Hydrochloric Acid → 4-Oxo-4,5,6,7-tetrahydrothieno-(3,2-C)pyridine
反応式
[O:1]=[C:2]1[C:7]2[CH:8]=[CH:9][S:10][C:6]=2[CH2:5][CH2:4][N:3]1C(=O)C.Cl>C(O)C>[O:1]=[C:2]1[C:7]2[CH:8]=[CH:9][S:10][C:6]=2[CH2:5][CH2:4][NH:3]1参加物
4
実験手順
An initially heterogeneous mixture of 4-oxo-5-acetyl-4,5,6,7-tetrahydro-thieno[3,2-c]pyridine (13.6 g; 0.069 mole) from Example 5, ethanol (50 ml) and 6 N hydrochloric acid (50 ml) is stirred for 4 hours at room temperature. The reaction mixture is concentrated in vacuo, the residue is made slightly basic by addition of sodium hydroxide and is then extracted with methylene chloride. The organic extracts are washed with water, dried over sodium sulfate and evaporated to dryness. The resulting residue is recrystallized from isopropanol-diisopropyl ether, to give white crystals, M.p.=94° C. Yield: 70%.
後処理
- concentrationThe reaction mixture is concentrated in vacuo
- additionthe residue is made slightly basic by addition of sodium hydroxide
- extractionis then extracted with methylene chloride
- washThe organic extracts are washed with water
- dry with materialdried over sodium sulfate
- customevaporated to dryness
- customThe resulting residue is recrystallized from isopropanol-diisopropyl ether
- customto give white crystals, M.p.=94° C
出典と根拠
- ORDレコード
- ord-aad55a20070d4e9fb55e43116e1f0c9c
- 出典データセット
- uspto-grants-1980_03
- 特許番号
- US04193997
反応ノート
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