Ammonium Hydroxide → 5-Pyrimidinecarboxylic acid, 4-amino-2-(methylthio)-, ethyl ester
반응식
[OH-].[NH4+:2].Cl[C:4]1[C:9]([C:10]([O:12][CH2:13][CH3:14])=[O:11])=[CH:8][N:7]=[C:6]([S:15][CH3:16])[N:5]=1>C(O)C>[NH2:2][C:4]1[C:9]([C:10]([O:12][CH2:13][CH3:14])=[O:11])=[CH:8][N:7]=[C:6]([S:15][CH3:16])[N:5]=1참가 물질
4
실험 절차
Add concentrated ammonium hydroxide (335 mL, 8.60 mol) to a vigorously stirred suspension of ethyl 4-chloro-2-(methylthio)pyrimidine-5-carboxylate (200 g, 860 mmol) in ethanol (EtOH) (450 mL) and allow to stir overnight. Collect the solids by filtration, rinse with EtOH (2×100 mL) and H2O (3×200 mL) and dry in a vacuum oven (65-70° C.) overnight to afford the title compound (164.4 g, 90% yield) as a white solid. MS (m/z): 214.1 (M+1).
후처리
- customCollect the solids
- filtrationby filtration
- washrinse with EtOH (2×100 mL) and H2O (3×200 mL)
- customdry in a vacuum oven (65-70° C.) overnight
출처 및 근거
- ORD 기록
- ord-4e58a5e0242642739bfd02531306943d
- 출처 데이터셋
- uspto-grants-2016_05
- 특허 번호
- US09334267B2
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