Hydrochloric Acid → HCID 22717664、化合物

HRID 1582541ノート

反応式

HRID 1582541 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

HCID 22717664HCID 22717664、化合物収率 43.5%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-27146999a9c6476d9c2e1b2691c75e24
出典データセット
uspto-grants-2004_05
特許番号
US06737382B1

反応ノート

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