HCID 13961960, 화합물 → HCID 178503558, 화합물
반응식
N([O-])=[O:2].[Na+].Cl[C:6]1[CH:11]=[C:10]([O:12][CH:13]([F:15])[F:14])[N:9]=[C:8]([S:16][CH3:17])[N:7]=1>CN(C)C=O>[F:14][CH:13]([F:15])[O:12][C:10]1[CH:11]=[C:6]([OH:2])[N:7]=[C:8]([S:16][CH3:17])[N:9]=1참가 물질
4
실험 절차
Over 50 minutes, a solution of 8.8 g (0.127 mole) of sodium nitrite in 10 ml of dimethylformamide is added dropwise at 140° C. to a solution of 8.7 g (0.038 mole) of 4-chloro-6-difluoromethoxy-2-methylthiopyrimidine in 10 ml of dimethylformamide. When the addition of the sodium nitrite is complete, the mixture is stirred for 2 hours at 140° to 150° C. The solvent is then evaporated off in vacuo and the residue is crystallised from 1N hydrochloric acid, affording 5.6 g (70% of theory) of 4-difluoromethoxy-6-hydroxy-2-methylthiopyrimidine with a melting point of 236°-237° C.
후처리
- customThe solvent is then evaporated off in vacuo
- customthe residue is crystallised from 1N hydrochloric acid
출처 및 근거
- ORD 기록
- ord-d2b6cc7673524f8a89b8382c16ec5160
- 출처 데이터셋
- uspto-grants-1987_09
- 특허 번호
- US04692524
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