تفاعل #56115

معادلة التفاعل

benzoyl cyanide

t-butanol

sulfuric acid

→

phenylglyoxylic-N-t-butylamide

المردود 95.0%

المذيبات

methylene chloride

ظروف التفاعل

المعالجة

1. 1
   أخرىThere were present in a stirrer
2. 2
   أخرىequipped apparatus
3. 3
   workup.STIRRINGAfter the end of the dropping, the mixture was post-stirred for another hour at room temperature
4. 4
   workup.STIRRINGwell agitated
5. 5
   استخلاصSubsequently, the mixture was extracted with methylene chloride
6. 6
   أخرىthe methylene chloride solution evaporated

الإجراء التجريبي

There were present in a stirrer equipped apparatus protected against moisture, 131 grams (1.0 mole) of benzoyl cyanide, 148 grams (2.0 moles) of t-butanol and 50 ml of methylene chloride and under stirring at about +50° C. it was treated by dropwise addition 150 grams (1.5 moles) of concentrated sulfuric acid. After the end of the dropping, the mixture was post-stirred for another hour at room temperature and then the entire mixture poured on 400 grams of ice and well agitated. Subsequently, the mixture was extracted with methylene chloride and the methylene chloride solution evaporated. There resulted 195 grams of phenylglyoxylic-N-t-butylamide which corresponds to a yield of 95% based on the acyl cyanide added. The amide has a melting point of 76°-77° C.

المصدر