반응 #343071

반응 방정식

crotononitrile

tetrahydrofuran

α-morpholino-α(4-morpholino-3-nitrophenyl)-acetonitrile

tetrahydrofuran

potassium hydroxide

→

4-(4-morpholino-3-nitrophenyl)-4-(cyano)-4-(morpholino)-3-methylbutyronitrile

용매

methanol

water

반응 조건

후처리

1. 1
   추출extracted with 4×250 parts by volume of ethyl acetate
2. 2
   건조The combined organic extracts are dried over magnesium sulphate
3. 3
   농축concentrated under vacuum
4. 4
   기타The resulting crude product is triturated with a mixture of 50 parts by volume of ethyl acetate and hexane
5. 5
   기타The solid product is collected
6. 6
   세척washed with ethyl acetate
7. 7
   기타dried at 80° under vacuum

실험 절차

A solution of 8.0 parts of crotononitrile in 20 parts by volume of tetrahydrofuran is added to a stirred mixture of 16.5 parts of α-morpholino-α(4-morpholino-3-nitrophenyl)-acetonitrile in 150 parts by volume of tetrahydrofuran and 1.5 parts of potassium hydroxide in 5 parts by volume of methanol at room temperature under an atmosphere of nitrogen. The reaction mixture is stirred for a further 6 hours, diluted with 500 parts by volume of water and extracted with 4×250 parts by volume of ethyl acetate. The combined organic extracts are dried over magnesium sulphate and concentrated under vacuum. The resulting crude product is triturated with a mixture of 50 parts by volume of ethyl acetate and hexane. The solid product is collected, washed with ethyl acetate and dried at 80° under vacuum to give 4-(4-morpholino-3-nitrophenyl)-4-(cyano)-4-(morpholino)-3-methylbutyronitrile having melting point 175°-177° C.

출처