HCID 3645909、化合物 → HCID 178435023、化合物
反応式
[Cl:1][C:2]1[N:3]=[C:4](Cl)[C:5]2[C:10]([CH3:11])=[C:9]([CH3:12])[S:8][C:6]=2[N:7]=1.[BH4-].[Na+]>C(O)C.C(Cl)(Cl)Cl>[Cl:1][C:2]1[NH:3][CH2:4][C:5]2[C:10]([CH3:11])=[C:9]([CH3:12])[S:8][C:6]=2[N:7]=1参加物
4
実験手順
To a solution of 4.66 g of 2,4-dichloro-5,6-dimethylthieno[2,3-d]pyrimidine in 150 ml of ethanol-chloroform (1:1 by volume) was slowly added 2.32 g of sodium borohydride with stirring. The mixture was stirred at room temperature for 6 hours and the solvent removed in vacuo. To the solid residue was added 50 ml of water and the insoluble material was filtered, washed with water, dried, and recrystallized from benzene to give 2.05 g of 2-chloro-5,6-dimethyl-3,4-dihydrothieno[2,3-d]pyrimidine, mp 170°-172° C.
後処理
- stirringThe mixture was stirred at room temperature for 6 hours
- customthe solvent removed in vacuo
- additionTo the solid residue was added 50 ml of water
- filtrationthe insoluble material was filtered
- washwashed with water
- customdried
- customrecrystallized from benzene
出典と根拠
- ORDレコード
- ord-4e42bcc474f14d85ae1c31f9f5806486
- 出典データセット
- uspto-grants-1981_08
- 特許番号
- US04284773
反応ノート
読み込み中…