Sodium Hydroxide → 2-(4-Chloro-phenyl)-4-(2,2-dimethoxy-ethyl)-thiazole-5-carboxylic acid

HRID 554840ノート

反応式

HRID 554840 の反応式
C[O:2][C:3]([C:5]1[S:9][C:8]([C:10]2[CH:15]=[CH:14][C:13]([Cl:16])=[CH:12][CH:11]=2)=[N:7][C:6]=1[CH2:17][CH:18]([O:21][CH3:22])[O:19][CH3:20])=[O:4].[OH-].[Na+]>CCO>[Cl:16][C:13]1[CH:14]=[CH:15][C:10]([C:8]2[S:9][C:5]([C:3]([OH:4])=[O:2])=[C:6]([CH2:17][CH:18]([O:21][CH3:22])[O:19][CH3:20])[N:7]=2)=[CH:11][CH:12]=1

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 674611542-(4-Chloro-phenyl)-4-(2,2-dimethoxy-ethyl)-thiazole-5-carboxylic acid methyl ester

生成物 1

HCID 674605292-(4-Chloro-phenyl)-4-(2,2-dimethoxy-ethyl)-thiazole-5-carboxylic acid収率 96%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
0 °C

実験手順

Mix 2-(4-chloro-phenyl)-4-(2,2-dimethoxy-ethyl)-thiazole-5-carboxylic acid methyl ester (3.6 g, 10.5 mmol) in EtOH (40 mL) and then add 2 M NaOH (6.8 mL). Stir the slurry mechanically overnight and then concentrate in vacuo. Dissolve the solid in water (40 mL), cool to 0° C., and adjust the pH to 5-6 with 1 N HCl (13 mL). Stir the slurry for 15 min, collect the precipitate, and wash the solid with water (4×20 mL). Dry the solid in a vacuum oven overnight to give 3.3 g (96%) of the title compound. ES/MS m/z (35Cl) 326.0 [M−1]−.

後処理

  1. concentrationconcentrate in vacuo
  2. dissolutionDissolve the solid in water (40 mL)
  3. stirringStir the slurry for 15 min
  4. customcollect the precipitate
  5. washwash the solid with water (4×20 mL)
  6. customDry the solid in a vacuum oven overnight

出典と根拠

ORDレコード
ord-5ec61726b0bb42b9ba82529618dd7266
出典データセット
uspto-grants-2011_11
特許番号
US08049013B2

反応ノート

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