반응식
[Cl:1][C:2]1[N:7]=[C:6]([NH:8][CH2:9][C:10]2[CH:11]=[N:12][N:13]([CH3:15])[CH:14]=2)[C:5]([C:16]([O:18]CC)=[O:17])=[CH:4][N:3]=1.[Li+].[OH-]>C1COCC1>[Cl:1][C:2]1[N:7]=[C:6]([NH:8][CH2:9][C:10]2[CH:11]=[N:12][N:13]([CH3:15])[CH:14]=2)[C:5]([C:16]([OH:18])=[O:17])=[CH:4][N:3]=1참가 물질
4
실험 절차
To a solution of give ethyl 2-chloro-4-((1-methyl-1H-pyrazol-4-yl)methylamino)pyrimidine-5-carboxylate (crude from step 1) in THF (9 mL), aq. 1N LiOH (6.6 mL, 6.6 mmol) was added. The mixture was stirred at room temperature overnight. THF was removed under vacuum, and the residue was acidified of with 1N HCl, the precipitated white solids were collected, and dried on vacuum to give 2-chloro-4-((1-methyl-1H-pyrazol-4-yl)methylamino)pyrimidine-5-carboxylic acid (1 g). MS 268.2, 270.2 (M+H, Cl pattern).
후처리
- customTHF was removed under vacuum
- customthe precipitated white solids were collected
- customdried on vacuum
출처 및 근거
- ORD 기록
- ord-1ec57e5fb192451db9597576c08fd45c
- 출처 데이터셋
- uspto-grants-2014_10
- 특허 번호
- US08853230B2
연결된 노트
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