Hydrochloric Acid → HCID 86642839、化合物

HRID 1667770ノート

反応式

HRID 1667770 の反応式
C([Si]([O:8][CH2:9][CH2:10][CH2:11][O:12][C:13]1[CH:18]=[C:17](F)[C:16]([N+:20]([O-:22])=[O:21])=[CH:15][C:14]=1[O:23][CH3:24])(C)C)(C)(C)C.[NH2:25][C:26]1[S:27][C:28]([C:38]([NH2:40])=[O:39])=[C:29]([C:31]2[CH:36]=[CH:35][CH:34]=[C:33]([Cl:37])[CH:32]=2)[N:30]=1.C(=O)([O-])[O-].[Cs+].[Cs+].Cl>O.CN(C)C=O>[Cl:37][C:33]1[CH:32]=[C:31]([C:29]2[N:30]=[C:26]([NH:25][C:17]3[CH:18]=[C:13]([O:12][CH2:11][CH2:10][CH2:9][OH:8])[C:14]([O:23][CH3:24])=[CH:15][C:16]=3[N+:20]([O-:22])=[O:21])[S:27][C:28]=2[C:38]([NH2:40])=[O:39])[CH:36]=[CH:35][CH:34]=1

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 10796Cesium carbonateHCID 166588232-Amino-4-(3-chlorophenyl)thiazole-5-carboxamideHCID 67428158Tert-butyl-[3-(5-fluoro-2-methoxy-4-nitro-phenoxy)-propoxy]-dimethyl-silane

生成物 1

HCID 86642839HCID 86642839、化合物収率 85.3%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

A mixture of 0.469 g (1.31 mmole) of tert-butyl-[3-(5-fluoro-2-methoxy-4-nitro-phenoxy)-propoxy]-dimethyl-silane (IV.42), 0.331 g (1.31 mmole) of 2-amino-4-(3-chloro-phenyl)-thiazole-5-carboxylic acid amide (V.2), 1.28 g (3.93 mmole) of cesium carbonate and 5 mL of dimethylformamide was heated at 70 degrees for 3 hours. The mixture was cooled and 3 mL of 6M hydrochloric acid was added dropwise. Stirring was continued for 15 minutes. The mixture was poured into 50 mL of water, and the precipitated orange solid was collected by filtration, washed with water, and air-dried to give 0.535 g of 4-(3-chloro-phenyl)-2-[5-(3-hydroxy-propoxy)-4-methoxy-2-nitro-phenylamino]-thiazole-5-carboxylic acid amide (VI.42).

後処理

  1. temperaturewas heated at 70 degrees for 3 hours
  2. temperatureThe mixture was cooled
  3. filtrationthe precipitated orange solid was collected by filtration
  4. washwashed with water
  5. customair-dried

出典と根拠

ORDレコード
ord-3aba5318ed1049ba9a0c45ee6f9510aa
出典データセット
uspto-grants-2011_10
特許番号
US08044213B2

反応ノート

読み込み中…