反応式
N1CCC[C@H]1[C:3]([C@H:5]1[CH2:9][CH2:8][CH2:7][NH:6]1)=O.Cl.[OH-].[Na+]>C1COCC1>[N:6]1([CH2:3][C@H:5]2[CH2:9][CH2:8][CH2:7][NH:6]2)[CH2:7][CH2:8][CH2:9][CH2:5]1参加物
5
反応条件
- 温度
- 0 °C
実験手順
2-(R)-Prolylpyrrolidine (1.2 g, 7.1 mmol) was dissolved in THF (10 ml). The reaction mixture was cooled to 0° C. and BH3, 1M in THF (10 ml, 10 mmol) was dropwise at 0 C. The reaction mixture was refluxed for 16 h, 3 M HCl (4.7 ml). 2 M NaOH solution was added until pH 10 was reached. The product was extracted with 5% MeOH in CH2Cl2 (three times). The organic layers were dried over Na2SO4 and the solvent was removed to provide the title compound as a slightly yellow liquid (73%), which was used without further purification for the next step.
後処理
- temperatureThe reaction mixture was refluxed for 16 h
- extractionThe product was extracted with 5% MeOH in CH2Cl2 (three times)
- dry with materialThe organic layers were dried over Na2SO4
- customthe solvent was removed
出典と根拠
- ORDレコード
- ord-ff3d358a37914d5692b06abcb1443767
- 出典データセット
- uspto-grants-2003_11
- 特許番号
- US06642232B2
関連ノート
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