Cesium carbonate → 2-(5-Dimethoxymethyl-2-nitro-phenylamino)-4-(3-trifluoromethyl-phenyl)-thiazole-5-carboxylic acid amide

HRID 1667793ノート

反応式

HRID 1667793 の反応式
[NH2:1][C:2]1[S:3][C:4]([C:17]([NH2:19])=[O:18])=[C:5]([C:7]2[CH:12]=[CH:11][CH:10]=[C:9]([C:13]([F:16])([F:15])[F:14])[CH:8]=2)[N:6]=1.[CH3:20][O:21][CH:22]([O:33][CH3:34])[C:23]1[CH:28]=[CH:27][C:26]([N+:29]([O-:31])=[O:30])=[C:25](F)[CH:24]=1.C(=O)([O-])[O-].[Cs+].[Cs+].[Cl-].[NH4+]>CN(C)C=O>[CH3:34][O:33][CH:22]([O:21][CH3:20])[C:23]1[CH:28]=[CH:27][C:26]([N+:29]([O-:31])=[O:30])=[C:25]([NH:1][C:2]2[S:3][C:4]([C:17]([NH2:19])=[O:18])=[C:5]([C:7]3[CH:12]=[CH:11][CH:10]=[C:9]([C:13]([F:16])([F:14])[F:15])[CH:8]=3)[N:6]=2)[CH:24]=1

参加物

6

反応物 4

HCID 10796Cesium carbonateHCID 25517Ammonium ChlorideHCID 540322924-Dimethoxymethyl-2-fluoro-1-nitrobenzeneHCID 593753582-Amino-4-(3-trifluoromethyl-phenyl)-thiazole-5-carboxylic acid amide

生成物 1

HCID 866428532-(5-Dimethoxymethyl-2-nitro-phenylamino)-4-(3-trifluoromethyl-phenyl)-thiazole-5-carboxylic acid amide収率 87.3%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A mixture of 0.5691 g (1.981 mmole) of 2-amino-4-(3-trifluoromethyl-phenyl)-thiazole-5-carboxylic acid amide (V.48), 0.4515 g (2.098 mmole) of 4-dimethoxymethyl-2-fluoro-1-nitro-benzene 29 mL of dimethylformamide and 3.2215 g (9.877 mmole) of cesium carbonate was heated at 56 degrees for 4 hours. The cooled mixture was poured into dilute aqueous ammonium chloride solution. The precipitate was collected by filtration, washed with water, and dried to give 0.8344 g of 2-(5-dimethoxymethyl-2-nitro-phenylamino)-4-(3-trifluoromethyl-phenyl)-thiazole-5-carboxylic acid amide (VI.48a) as a brown-orange solid.

後処理

  1. temperaturewas heated at 56 degrees for 4 hours
  2. filtrationThe precipitate was collected by filtration
  3. washwashed with water
  4. customdried

出典と根拠

ORDレコード
ord-fc67063a8c5644a8b8b956116a7b4d23
出典データセット
uspto-grants-2011_10
特許番号
US08044213B2

反応ノート

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