4-Methylbenzoyl Chloride → 5-(4-Toluamido)-3-Trichloromethyl-1,2,4-Thiadiazole

HRID 66937

반응식

HRID 66937 반응식
[NH2:1][C:2]1[S:6][N:5]=[C:4]([C:7]([Cl:10])([Cl:9])[Cl:8])[N:3]=1.[C:11]1([CH3:20])[CH:16]=[CH:15][C:14]([C:17](Cl)=[O:18])=[CH:13][CH:12]=1>C1(C)C=CC=CC=1>[C:11]1([CH3:20])[CH:16]=[CH:15][C:14]([C:17]([NH:1][C:2]2[S:6][N:5]=[C:4]([C:7]([Cl:10])([Cl:9])[Cl:8])[N:3]=2)=[O:18])=[CH:13][CH:12]=1

참가 물질

4

반응물 2

HCID 134054-Methylbenzoyl ChlorideHCID 6028483-(Trichloromethyl)-1,2,4-thiadiazol-5-amine

생성물 1

HCID 130415165-(4-Toluamido)-3-Trichloromethyl-1,2,4-Thiadiazole

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

A solution of 11.0 g (0.05 mole) 5-amino-3-trichloromethyl-1,2,4-thiadiazole and 8.0 g (0.05 mole) 4-toluoyl chloride in 250 ml toluene was heated at reflux for 20 hours. Unreacted amino compound was removed by cooling the reaction mixture and filtering the precipitate. Concentration of the filtrate in vacuo gave the crude product, which was purified by recrystallization from cyclohexane. Yield was 9.1 g (27%); m.p. 127° C.

후처리

  1. temperatureat reflux for 20 hours
  2. customUnreacted amino compound was removed
  3. temperatureby cooling the reaction mixture
  4. filtrationfiltering the precipitate

출처 및 근거

ORD 기록
ord-941fe4c55371425b876f0a5cbd9052c1
출처 데이터셋
uspto-grants-1982_08
특허 번호
US04343945

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