HCID 13961960、化合物 → HCID 178503558、化合物
反応式
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]=1参加物
4
実験手順
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.
後処理
- customThe solvent is then evaporated off in vacuo
- customthe residue is crystallised from 1N hydrochloric acid
出典と根拠
- ORDレコード
- ord-d2b6cc7673524f8a89b8382c16ec5160
- 出典データセット
- uspto-grants-1987_09
- 特許番号
- US04692524
反応ノート
読み込み中…