Formaldehyde → (R)-Methyl 1-methylpyrrolidine-2-carboxylate
反応式
[CH3:1][O:2][C:3](=[O:9])[C@H:4]1[CH2:8][CH2:7][CH2:6][NH:5]1.[CH2:10]=O>CN(C=O)C>[CH3:1][O:2][C:3](=[O:9])[C@H:4]1[CH2:8][CH2:7][CH2:6][N:5]1[CH3:10]参加物
4
実験手順
(2R)-proline methylester (1.20 g, 10.0 mmol) was dissolve in DMF (30 mL), and formalin (37% in water, 1.12 mL, 15.0 mmol) and NaBH (OAc)3 (4.20 g, 20.0 mmol) were added portionwise. After 12 h, the reaction material was concentrated in vacuo, and the residue was diluted with NaHCO3 (30 mL). The organic material was extracted with EtOAc, and the organic extracts were dried over MgSO4 and concentrated in vacuo. The residue was purified by column chomatography (EtOAc/Hex=4/1) to give the title compound (1.33 g, 93.0%).
後処理
- concentrationthe reaction material was concentrated in vacuo
- additionthe residue was diluted with NaHCO3 (30 mL)
- extractionThe organic material was extracted with EtOAc
- dry with materialthe organic extracts were dried over MgSO4
- concentrationconcentrated in vacuo
- customThe residue was purified by column chomatography (EtOAc/Hex=4/1)
出典と根拠
- ORDレコード
- ord-eb3a8e91ebaa468084ee19832f0d7f82
- 出典データセット
- uspto-grants-2011_08
- 特許番号
- US07989634B2
反応ノート
読み込み中…