반응 #981280

반응 방정식

benzoyl chloride

thiocarbohydrazide

water

→

1,5-bisbenzoyl-thiocarbohydrazide

용매

pyridine

반응 조건

후처리

1. 1
   온도cooling
2. 2
   workup.ADDITIONAfter addition
3. 3
   workup.STIRRINGthe mixture is stirred for a further 3 hours at room temperature
4. 4
   기타The precipitate obtained
5. 5
   기타is separated
6. 6
   workup.DISSOLUTIONdissolved
7. 7
   기타reprecipitated from methanol/water
8. 8
   기타after drying in air
9. 9
   workup.ADDITIONis mixed with 1.7 liters of boiling ethyl acetate
10. 10
    온도after cooling
11. 11
    여과filtered
12. 12
    기타dried in the air

실험 절차

116 ml of benzoyl chloride are added dropwise at a temperature of 25° C. to a suspension of 53 g of thiocarbohydrazide in 350 ml of pyridine with stirring and cooling. After addition, the mixture is stirred for a further 3 hours at room temperature and subsequently mixed with 6 liters of water. The precipitate obtained is separated, dissolved and reprecipitated from methanol/water and, after drying in air is mixed with 1.7 liters of boiling ethyl acetate and after cooling, is suction filtered and dried in the air. 112 g of 1,5-bisbenzoyl-thiocarbohydrazide which melts at 177° to 179° C. with decomposition are obtained.

출처