반응식
[NH2:1][C:2]1[N:7]=[C:6]([C:8]2[CH:13]=[CH:12][C:11]([Cl:14])=[CH:10][CH:9]=2)[N:5]=[C:4]([C:15]([OH:17])=[O:16])[C:3]=1[Cl:18].S(Cl)(Cl)=O.O.[OH-].[Na+].[CH2:26](O)[CH3:27]>>[NH2:1][C:2]1[N:7]=[C:6]([C:8]2[CH:13]=[CH:12][C:11]([Cl:14])=[CH:10][CH:9]=2)[N:5]=[C:4]([C:15]([O:17][CH2:26][CH3:27])=[O:16])[C:3]=1[Cl:18]참가 물질
6
실험 절차
To a solution of 6-amino-5-chloro-2-(4-chlorophenyl)-4-pyrimidinecarboxylic acid (i.e. the product of Example 4, Step C) (20.0 g, 70.4 mmol) in ethanol (70 mL) was added thionyl chloride (5.14 mL, 70.4 mmol) while maintaining the temperature below 15° C. using an ice bath. The reaction mixture was then heated at reflux overnight. Water was added. Then with external cooling aqueous sodium hydroxide (50%) was added to adjust the pH to 7. The resulting solid was isolated by filtration and dried to afford the title product, a compound of the present invention, as a light beige solid (20.1 g).
후처리
- temperaturewhile maintaining the temperature below 15° C.
- temperatureThe reaction mixture was then heated
- temperatureat reflux overnight
- customThe resulting solid was isolated by filtration
- customdried
출처 및 근거
- ORD 기록
- ord-3a5274efcd154ce9bcc39c6ca0997ed0
- 출처 데이터셋
- uspto-grants-2015_09
- 특허 번호
- US09144240B2
연결된 노트
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