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

HRID 554840노트

반응식

HRID 554840 반응식
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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
0 °C

실험 절차

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]−.

후처리

  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

출처 및 근거

ORD 기록
ord-5ec61726b0bb42b9ba82529618dd7266
출처 데이터셋
uspto-grants-2011_11
특허 번호
US08049013B2

반응 노트

불러오는 중…