2,4-Dichlorobenzoyl chloride → 5-(2,4-Dichlorobenzamido)-3-Trichloromethyl-1,2,4-Thiadiazole

HRID 66945노트

반응식

HRID 66945 반응식
[NH2:1][C:2]1[S:6][N:5]=[C:4]([C:7]([Cl:10])([Cl:9])[Cl:8])[N:3]=1.[Cl:11][C:12]1[CH:20]=[C:19]([Cl:21])[CH:18]=[CH:17][C:13]=1[C:14](Cl)=[O:15]>C1(C)C(C)=CC=CC=1>[Cl:11][C:12]1[CH:20]=[C:19]([Cl:21])[CH:18]=[CH:17][C:13]=1[C:14]([NH:1][C:2]1[S:6][N:5]=[C:4]([C:7]([Cl:10])([Cl:9])[Cl:8])[N:3]=1)=[O:15]

참가 물질

4

반응물 2

HCID 666452,4-Dichlorobenzoyl chlorideHCID 6028483-(Trichloromethyl)-1,2,4-thiadiazol-5-amine

생성물 1

HCID 130415245-(2,4-Dichlorobenzamido)-3-Trichloromethyl-1,2,4-Thiadiazole수율 69.5%

시약·촉매·용매 1

HCID 7237O-Xylene용매

실험 절차

A solution of 10.9 g (0.05 mole) 5-amino-3-trichloromethyl-1,2,4-thiadiazole and 20.9 g (0.10 mole) 2,4-dichlorobenzoyl chloride was refluxed in 200 ml xylene for 20 hours. The reaction mixture was concentrated in vacuo and the resulting residue extracted with benzene. Addition of hexane resulted in precipitation of 13.6 g (69% yield) pure product; m.p. 136° C.

후처리

  1. concentrationThe reaction mixture was concentrated in vacuo
  2. extractionthe resulting residue extracted with benzene
  3. additionAddition of hexane

출처 및 근거

ORD 기록
ord-5ed551a71a4646b6861ec463374c3df0
출처 데이터셋
uspto-grants-1982_08
특허 번호
US04343945

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