Chapter 438: "Joule", AM text


Xu Qiu and Han Jiaying joined hands and walked into the organic laboratory on the fifth floor.
After a few months, Xu Qiu really missed the smell of the familiar solvent again. He was very proficient in wearing protective equipment such as lab coat, three-layer protective gloves, and disposable activated carbon mask.
These basic experimental skills have long become muscle memory.
Xu Qiu didn't wear the gas mask. It was too much trouble to wear, and the experiment to be carried out today is not dangerous.
The synthesis steps of PTQ1 are relatively simple, only three steps are required:
In the first step, "3,6-dibromo-4,5-difluorobenzene-1,2-diamine", referred to as "hexasubstituted benzene", is reacted with glyoxylic acid and acetic acid at room temperature to remove the benzene ring The two amino groups above are cyclized into a six-membered heterocyclic ring, that is, 1,4-azabenzene, thereby obtaining a condensed ring structure formed by benzene and 1,4-azabenzene.
In the second step, the product obtained in the first step is reacted with 1-bromo-2-hexyldecane under the action of potassium tert-butoxide. The purpose is to introduce alkoxy side chains to obtain monomers for polymerization. Body unit. This type of unit is the A unit that tends to attract electrons and was named Q by Xu Qiu, mainly because the shape of its molecular structure is very similar to the letter Q.
In the third step, the bis-bromo-substituted Q unit and the bis-trimethyltin-substituted thiophene unit T are subjected to a Stille coupling reaction to obtain the conjugated polymer donor material PTQ1.
The PTQ series donors, because of their relatively simple structure, can be controlled only by the side chain of the alkoxy group attached to 1,4-Azepine, and a free reaction site next to the side chain.
For example, the vacant reaction site on the PTQ1 material is a hydrogen atom, which can be replaced with various other groups, such as a methyl group, a fluorine atom, a chlorine atom, and another side chain. This is what the school girl will be responsible for afterwards.
Xu Qiu and Han Jiaying each occupy an adjacent fume hood and plan to cast the same reaction separately.
In fact, Han Jiaying's experimental skills in the synthesis of body materials are no longer weaker than Xu Qiu's. The proficiency of the two has reached the fifth level, and the gap is not big.
It is not so much that Xu Qiu is guiding Han Jiaying, it is better to say that it is safer to combine two people together, as long as there is no problem with the raw materials, and the probability of the experiment failure is too low.
As for why Xu Qiu didn't directly give this job to the school girl, it was because he also wanted to warm up, and then he had to synthesize Y series receptors.
If he doesn't do experiments on the front line for a long time, the probability of success of the synthesis reaction will be reduced. He doesn't want to delay too much time due to the failure of the experiment when synthesizing Y series receptors.
Start the experiment.
Xu Qiu first took a clean two-necked flask, and then added 906 mg of hexasubstituted benzene, 222 mg of glyoxylic acid, and 30 ml of acetic acid to the inside. Then, the mixture was heated to 40 degrees Celsius. After 10 minutes, The solution was returned to room temperature and stirring was continued for 3 hours.
This step of the experiment is relatively simple, no need to re-evaporate the solvent, just use the purchased raw materials directly.
Among them, it involves a new material-glyoxylic acid.
Glyoxylic acid is a white crystal with a melting point of about 98 degrees Celsius. It is an intermediate of medicines, dyes, plastics and pesticides. It has low toxicity. According to the MSDS manual, it emits an unpleasant odor.
However, when Xu Qiu weighed glyoxylic acid through a fume hood, he did not smell any special smell.
In contrast, the taste of acetic acid is more pungent and full of vinegar.
It is also easy to understand. After all, acetic acid is a liquid and it is easier to evaporate.
At noon, the three of them went to Jiangwan Canteen for lunch.
Now the second floor of the canteen on the Jiangwan side is open, the quality of the dishes has indeed been slightly improved, and there are more types to choose from, including fried rice, fried noodles, fried rice noodles, spicy hot pot, and yellow braised chicken rice. , Huang Braised Short Ribs and other dishes.
In the afternoon, after the reaction was completed, Xu Qiu used a Buchner funnel to filter and collect the precipitates obtained from the reaction, and dried them in a vacuum oven to obtain a large amount of white solids.
Xu Qiu weighed the crude product, which was 1.1 g. The yield of this reaction was not low.
Taking into account the side reaction products of this step and the remaining small amount of raw materials will not affect the next step of the reaction, Xu Qiu directly weighed 1 gram of the white solid just obtained, and combined it with 395 mg of tert-butyl Mix potassium alkoxide and 897 mg of 1-bromo-2-hexyldecane and dissolve in 30 ml of methanol solvent.
The role of 1-bromo-2-hexyldecane is to introduce side chains.
Potassium tert-butoxide is an important organic base used to provide a basic reaction environment. Its alkalinity is stronger than that of potassium hydroxide, and the alkalinity of potassium hydroxide is stronger than that of sodium hydroxide. Sodium is very common, it is caustic soda.
Here, Xu Qiu once again remembered the chicken paws poisoned by sodium hydroxide solution in middle school.
The reaction in this step is not difficult. It only needs to react for 12 hours under the conditions of heating and reflux at 90 degrees Celsius. Today, there is definitely no way to deal with the reaction. You can only wait until tomorrow morning.
In his free time, Xu Qiu plans to purchase raw materials for the synthesis of Y series receptors, including dibromo-substituted NT units and monotrimethyltin-substituted TT units.
The first thing he thought of was the Blue River Optoelectronics Material Company, which he participated in, so he contacted Yang Qin, and the other party told Xu Qiu embarrassingly that the things he wanted were out of stock.
However, Yang Qin brought good news: "Ma Weiwei's research group from Ancheng Jiaotong University purchased one gram of -4F and one gram of ITIC-4F, and two other research groups also purchased some materials, although both Only one or two hundred milligrams of the "poor group" was purchased at a time, but it was a good start."
"In addition, the company recently recruited a master student and an undergraduate student, and the team has also begun to grow."
No matter what, the materials still have to be bought. If my company is out of stock, I can only find the Shenzhen Optoelectronics Co.
Xu Qiu opened the door and asked: "I want to buy a dibromo-substituted NT unit and a monotrimethyltin-substituted TT unit. The product numbers are NT7 and TT10, and 500 mg each."
Sales quickly replied: "NT7 is 2200 per gram, TT10 is 1200 per gram, and the price of 500 mg is 1200 and 700 respectively. If there is no problem, let the warehouse adjust the goods here."
Xu Qiu: "No problem."
Sales: "My dear, why didn't you come here to get the goods recently? We have newly released -4F and IDIC, and the efficiency can be more than 12%. Do you want to know, if you don't need finished products, we also have monomers. Sell ​​it."
Sales: "[November Hottest Product.jpg]"
Xu Qiu: "..."
This book is organized and produced by the public account. Follow VX [Book Friends Base Camp~EbookFREE.me~ to receive cash red envelopes!
Xu Qiu: "Do you share QQ accounts for your work?"
Sales: "Yeah."
Xu Qiu: "These two materials were developed by our group."
Sales: "Ah, excuse me."
Sales: "The goods here have been packaged for you, and the express delivery can be delivered today. Please have a happy life and scientific research smoothly."
Xu Qiu: "OK"
It is true that Xu Qiu from Shencheng Optoelectronics Company has not been patronizing for a long time, including now that the other party’s name is not included in the article, but the name of Blue River Optoelectronics Materials Co., Ltd. is used to promote his company.
Blue River heard that the Deep City Optoelectronics Company issued a bonus, and immediately said that our side did the same, and the bonus amount was 1.5 times theirs, and told Yang Qin of this bonus rule to let him promote it.
Therefore, the bonus for each article of Organic Photovoltaic in the group has not decreased but increased.
In the evening, Xu Qiu took Han Jiaying and Wu Shengnan to eat a bowl of Jiangwan's braised beef noodles, gave the treasure shop Amway to the two, and finally received unanimous praise from the two girls.
Although the Jiangwan Canteen is renovated and re-contracted, the quality of the dishes is good, but compared to the previous one, if compared with the Handan campus, it is even inferior to the southern canteen, and it is not as good as the headquarters and the north canteen. .
It can be said that "Jiangwan people's bitter canteen has been going on for a long time." Xu Qiu estimated that after the graduate students of science and engineering moved over, the canteen here will probably be rectified again.
On Tuesday morning, Xu Qiu came to the Jiangwan laboratory to deal with the reaction. He poured the reaction mixture into a saturated ammonium chloride solution, then extracted it with dichloromethane, and then washed it with water, repeated three times.
The obtained organic extract is added with anhydrous magnesium sulfate to dry, then filtered, and the solvent is evaporated to dryness by rotary evaporation to obtain a crude reaction product.
In most cases, the reaction product was a solid powder, but this time the crude product is unique and is a colorless oily product.
Originally, Xu Qiu thought that he hadn't done synthesis after a few months, and his strength had declined, causing the experiment to fail.
Later, I was relieved to see that the products obtained by the school girl were the same as him.
Two people get the same result, there is a high probability that there is no problem.
It's like when two Xueba take the exam and find the answers to all the questions are the same, it's mostly stable, and both of them are full marks.
And if two students finish the exam and find the answers to all the questions are the same, it will be a little scary...
Next, the crude product is passed through the column for further purification to obtain the final product.
The yield of this reaction is very high~EbookFREE.me~Xu Qiu's yield is 91%, and Han Jiaying's is also 90%.
The main difficulty in the synthesis of PTQ1 lies in the Q unit, and the subsequent reaction between the Q unit and the T unit is a simple Stille coupling reaction.
Therefore, Xu Qiu did not intend to participate in the next synthesis, and his hands are now hot, so he began to concentrate on the writing of "Joule" articles.
However, on Wednesday, Xu Qiu still ran to the Jiangwan campus, pretending that he was doing an experiment, he also tasted the sweetness.
Teacher Wei is usually on the Handan campus. He often makes inspections in the 216 laboratory and arrests people. He will call for inquiries only for very important matters.
It's really cool to stay away from Wei Xingsi and stay in Jiangwan now, and generally won't get caught.
On Thursday morning, when Xu Qiu was in class, he suddenly received a call from Wei Xingsi. After he hung up, he was about to send a text message. Wei Xingsi called again. After hanging up again, Wei Xingsi took the initiative to send a text message:
"The comments on "Joule" and AM's articles came over at the same time. I will forward the email to you immediately."
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