Methanol → methyl 6,7-dihydro-5H-cyclopenta[b]pyridine-6-carboxylate
反応式
Cl.[N:2]1[C:10]2[CH2:9][CH:8]([C:11]([OH:13])=[O:12])[CH2:7][C:6]=2[CH:5]=[CH:4][CH:3]=1.[CH3:14]O>S(=O)(=O)(O)O>[CH3:14][O:12][C:11]([CH:8]1[CH2:9][C:10]2[N:2]=[CH:3][CH:4]=[CH:5][C:6]=2[CH2:7]1)=[O:13]参加物
4
実験手順
A solution 6,7-dihydro-5H-[1]pyrindine-6-carboxylic acid hydrochloride (Example 88; 0.640 g, 3.21 mmol) and concentrated sulphuric acid (3 drops) in methanol (100 ml) is heated to reflux for 3 hours. The solvent is evaporated, the residue is treated with saturated aqueous NaHCO3 and extracted with EtOAc. The combined organic phases are washed with brine, dried (MgSO4) and evaporated to afford 6,7-dihydro-5H-[1]pyrindine-6-carboxylic acid methyl ester, MH+178.
後処理
- temperatureto reflux for 3 hours
- customThe solvent is evaporated
- additionthe residue is treated with saturated aqueous NaHCO3
- extractionextracted with EtOAc
- washThe combined organic phases are washed with brine
- dry with materialdried (MgSO4)
- customevaporated
出典と根拠
- ORDレコード
- ord-2c0cd0bc50d447c498c33c72bc4f4d4d
- 出典データセット
- uspto-grants-2010_06
- 特許番号
- US07745462B2
反応ノート
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