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

HRID 66936

반응식

HRID 66936 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][CH:14]=[C:13]([C:17](Cl)=[O:18])[CH:12]=1>C1(C)C(C)=CC=CC=1>[C:11]1([CH3:20])[CH:16]=[CH:15][CH:14]=[C:13]([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:12]=1

참가 물질

4

반응물 2

HCID 743753-Methylbenzoyl chlorideHCID 6028483-(Trichloromethyl)-1,2,4-thiadiazol-5-amine

생성물 1

HCID 130415155-(3-Toluamido)-3-Trichloromethyl-1,2,4-Thiadiazole수율 12%

시약·촉매·용매 1

HCID 7237O-Xylene용매

실험 절차

A solution of 22.0 g (0.1 mole) 5-amino-3-trichloromethyl-1,2,4-thiadiazole and 16.0 g (0.1 mole) 3-toluoyl chloride in 250 ml xylene was heated at reflux for 20 hours. The reaction mixture was cooled to room temperature and the resulting precipitate removed by filtration. The crude product was washed with petroleum ether and then recrystallized twice from toluene to obtain 4.0 g (12% yield) of pure product; m.p. 142° C.

후처리

  1. temperatureat reflux for 20 hours
  2. customthe resulting precipitate removed by filtration
  3. washThe crude product was washed with petroleum ether
  4. customrecrystallized twice from toluene

출처 및 근거

ORD 기록
ord-0ee1bf474793456ab285a40aa7291cc3
출처 데이터셋
uspto-grants-1982_08
특허 번호
US04343945

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