Ammonia → Methyl 6-amino-2-chloropyrimidine-4-carboxylate
반응식
[CH3:1][O:2][C:3]([C:5]1[CH:10]=[C:9](S(C)(=O)=O)[N:8]=[C:7]([Cl:15])[N:6]=1)=[O:4].[NH3:16]>O1CCOCC1.CO>[CH3:1][O:2][C:3]([C:5]1[CH:10]=[C:9]([NH2:16])[N:8]=[C:7]([Cl:15])[N:6]=1)=[O:4]참가 물질
5
실험 절차
2-Chloro-6-methanesulfonylpyrimidine-4-carboxylic acid methyl ester (3.7 g, 14.75 mmol) was dissolved in dioxane and 7N ammonia in methanol was added. The reaction mixture was stirred at room temperature for 3 hours, concentrated under vacuum, and the residue partitioned between ethyl acetate and water. The organic phase was dried and concentrated. The product was purified by column chromatography to provide 6-amino-2-chloropyrimidine-4-carboxylic acid methyl ester (2.35 g, 85% yield): 1H NMR (DMSO-d6): δ 7.6 (br s, 1H), 7.00 (s, 1H), 3.84 (s, 3H), 3.33 (s, 3H).
후처리
- concentrationconcentrated under vacuum
- customthe residue partitioned between ethyl acetate and water
- customThe organic phase was dried
- concentrationconcentrated
- customThe product was purified by column chromatography
출처 및 근거
- ORD 기록
- ord-66fb0aa808b34c818b7117d066569607
- 출처 데이터셋
- uspto-grants-2009_05
- 특허 번호
- US07538214B2
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