반응 #1604376

반응 방정식

1-(4-amino-3-nitrophenyl)-2-bromopropan-1-one

O-ethyl hydrazinecarbothioate

→

5-(4-amino-3-nitrophenyl)-6-methyl-3,6-dihydro-2H-1,3,4-thiadiazin-2-one

용매

acetonitrile

반응 조건

후처리

1. 1
   온도are refluxed for 4 hours
2. 2
   온도The reaction mixture is cooled
3. 3
   여과The crystalline solid is filtered off
4. 4
   세척washed with cold acetonitrile
5. 5
   기타to give
6. 6
   기타after drying

실험 절차

36.5 g (134 mM) of 1-(4-amino-3-nitrophenyl)-2-bromopropan-1-one and 24.3 g (202.5 mM) of O-ethyl hydrazinecarbothioate dissolved in 190 ml of acetonitrile are refluxed for 4 hours with stirring. The reaction mixture is cooled and maintained at 0° C. for 16 hours. The crystalline solid is filtered off and washed with cold acetonitrile to give, after drying, 10.4 g of 5-(4-amino-3-nitrophenyl)-6-methyl-3,6-dihydro-2H-1,3,4-thiadiazin-2-one in the form of a solid.

출처