3,5-Dinitrobenzoyl chloride → 5-(3,5-Dinitrobenzamido)-3-Trichloromethyl-1,2,4-Thiadiazole

HRID 66941

반응식

HRID 66941 반응식
[NH2:1][C:2]1[S:6][N:5]=[C:4]([C:7]([Cl:10])([Cl:9])[Cl:8])[N:3]=1.[N+:11]([C:14]1[CH:15]=[C:16]([CH:20]=[C:21]([N+:23]([O-:25])=[O:24])[CH:22]=1)[C:17](Cl)=[O:18])([O-:13])=[O:12]>C1(C)C=CC=CC=1>[N+:11]([C:14]1[CH:15]=[C:16]([CH:20]=[C:21]([N+:23]([O-:25])=[O:24])[CH:22]=1)[C:17]([NH:1][C:2]1[S:6][N:5]=[C:4]([C:7]([Cl:10])([Cl:9])[Cl:8])[N:3]=1)=[O:18])([O-:13])=[O:12]

참가 물질

4

반응물 2

HCID 74323,5-Dinitrobenzoyl chlorideHCID 6028483-(Trichloromethyl)-1,2,4-thiadiazol-5-amine

생성물 1

HCID 130415205-(3,5-Dinitrobenzamido)-3-Trichloromethyl-1,2,4-Thiadiazole수율 85%

시약·촉매·용매 1

HCID 1140Toluene용매

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온도
-10 °C

실험 절차

A solution of 10.9 g (0.05 mole) 5-amino-3-trichloromethyl-1,2,4-thiadiazole and 12.6 g (0.055 mole) 3,5-dinitrobenzoyl chloride in 200 ml toluene was refluxed for 20 hours. The crude product precipitated from the reaction mixture upon cooling to -10° C. After isolation by filtration, the residue was washed with hot petroleum ether and finally recrystallized from methylene chloride to give 17.5 g (85% yield) of pure product; m.p. 197° C.

후처리

  1. customThe crude product precipitated from the reaction mixture
  2. filtrationAfter isolation by filtration
  3. washthe residue was washed with hot petroleum ether
  4. customfinally recrystallized from methylene chloride

출처 및 근거

ORD 기록
ord-8e93b465b8fa4b39bec5f67f154ba6ef
출처 데이터셋
uspto-grants-1982_08
특허 번호
US04343945

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