Benzoyl chloride, 3-nitro- → 5-(3-Nitrobenzamido)-3-Trichloromethyl-1,2,4-Thiadiazole

HRID 66939

반응식

HRID 66939 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]=[CH:21][CH:22]=1)[C:17](Cl)=[O:18])([O-:13])=[O:12]>C1(C)C(C)=CC=CC=1>[N+:11]([C:14]1[CH:15]=[C:16]([CH:20]=[CH:21][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 8495Benzoyl chloride, 3-nitro-HCID 6028483-(Trichloromethyl)-1,2,4-thiadiazol-5-amine

생성물 1

HCID 130415185-(3-Nitrobenzamido)-3-Trichloromethyl-1,2,4-Thiadiazole수율 69.1%

시약·촉매·용매 1

HCID 7237O-Xylene용매

실험 절차

A solution of 21.8 g (0.1 mole) 5-amino-3-trichloromethyl-1,2,4-thiadiazole and 18.6 g (0.1 mole) 3-nitrobenzoyl chloride in 250 ml xylene was heated at reflux for 20 hours. Unreacted starting amino compound was recovered by cooling the reaction mixture and filtering the resulting precipitate. The filtrate was concentrated in vacuo and the residue recrystallized from xylene. After washing with petroleum ether, 25.4 g (69% yield) of pure product was obtained; m.p. 198° C.

후처리

  1. temperatureat reflux for 20 hours
  2. customUnreacted starting amino compound was recovered
  3. temperatureby cooling the reaction mixture
  4. filtrationfiltering the resulting precipitate
  5. concentrationThe filtrate was concentrated in vacuo
  6. customthe residue recrystallized from xylene
  7. washAfter washing with petroleum ether

출처 및 근거

ORD 기록
ord-de6e7a9e35cd4ea48025e0a704ebed64
출처 데이터셋
uspto-grants-1982_08
특허 번호
US04343945

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