반응 #215148

반응 방정식

1-phenyl-2-(3-sulfamoyl-4-chlorobenzoyl)-hydrazine

potassium iodide

allyl bromide

→

compound

1-Allyl-1-phenyl-2-(3-sulfamoyl-4-chlorobenzoyl)-hydrazine

용매

isopropanol

반응 조건

후처리

1. 1
   기타In a three necked 12 liter round bottom reaction flask equipped with a mechanical stirrer
2. 2
   온도reflux condenser
3. 3
   온도at gentle reflux for about 20 hours
4. 4
   여과suction filtered while still hot
5. 5
   세척The cake was washed with isopropanol 300 ml
6. 6
   세척the combined filtrate and wash
7. 7
   workup.ADDITIONwere diluted with warm water 2.7 liters
8. 8
   기타Crystallization
9. 9
   여과The crystals were filtered
10. 10
    세척washed with isopropanol-water (70% v/v)

실험 절차

In a three necked 12 liter round bottom reaction flask equipped with a mechanical stirrer and reflux condenser was placed isopropanol 6.1 liters and 1-phenyl-2-(3-sulfamoyl-4-chlorobenzoyl)-hydrazine 1.3 kg (4.1 mol), potassium iodide 68.0 g (0.41 mol) and allyl bromide 768 g (8 mol). This mixture was stirred at gentle reflux for about 20 hours then suction filtered while still hot. The cake was washed with isopropanol 300 ml and the combined filtrate and wash were diluted with warm water 2.7 liters. Crystallization occured in about 0.5 hours. The crystals were filtered and washed with isopropanol-water (70% v/v) to provide the compound (m.p. 99°-101° C.).

출처