Hydrochloric Acid → HCID 22717664, 화합물

HRID 1582541노트

반응식

HRID 1582541 반응식
[NH2:1][C:2]1[S:3][C:4]([Cl:11])=[C:5]([C:7]([F:10])([F:9])[F:8])[N:6]=1.[Cl:12][C:13]1[CH:21]=[CH:20][C:16]([C:17](Cl)=[O:18])=[CH:15][C:14]=1[N+:22]([O-:24])=[O:23].Cl>N1C=CC=CC=1>[Cl:11][C:4]1[S:3][C:2]([NH:1][C:17](=[O:18])[C:16]2[CH:20]=[CH:21][C:13]([Cl:12])=[C:14]([N+:22]([O-:24])=[O:23])[CH:15]=2)=[N:6][C:5]=1[C:7]([F:10])([F:8])[F:9]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 1234774-Chloro-3-nitrobenzoyl chlorideHCID 1781935-Chloro-4-(trifluoromethyl)-1,3-thiazol-2-amine

생성물 1

HCID 22717664HCID 22717664, 화합물수율 43.5%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

2-Amino-5-chloro-4-trifluoromethylthiazole (1.0 g) was dissolved in pyridine (5 ml) and 4-chloro-3-nitrobenzoylchloride (1.1 g) was added at room temperature with stirring. The mixture was stirred for 1 day at room temperature. The mixture was poured into ice water and acidified with aqueous hydrochloric acid then extracted with chloroform. The chloroform layer was dried over magnesium sulfate and the solvent was removed under reduced pressure. The solid thus obtained was recrystallized from methanol to give N-(5-chloro-4-trifluoromethylthiazol-2-yl)-4-chloro-3-nitro-benzamide (0.83 g), m. p. 183-184° C.

후처리

  1. stirringThe mixture was stirred for 1 day at room temperature
  2. extractionthen extracted with chloroform
  3. dry with materialThe chloroform layer was dried over magnesium sulfate
  4. customthe solvent was removed under reduced pressure
  5. customThe solid thus obtained
  6. customwas recrystallized from methanol

출처 및 근거

ORD 기록
ord-27146999a9c6476d9c2e1b2691c75e24
출처 데이터셋
uspto-grants-2004_05
특허 번호
US06737382B1

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