Water → HCID 20763143、化合物
反応式
C(O[C:6](=O)[NH:7][CH2:8][CH2:9][CH2:10][NH:11][CH2:12][CH2:13][OH:14])(C)(C)C.O>C1COCC1>[CH3:6][NH:7][CH2:8][CH2:9][CH2:10][NH:11][CH2:12][CH2:13][OH:14]参加物
4
実験手順
To a solution of [3-(2-Hydroxy-ethylamino)-propyl]-carbamic acid tert-butyl ester (900 mg, 4.1 mmol) in THF (20 mL) was added a 1M solution of BH3 in THF. The mixture was refluxed for 24 hours under nitrogen. The reaction was allowed to cool down and water (5 mL) was carefully added with vigorous stirring. The reaction mixture was concentrated to low volume and treated with a 6M aqueous solution of HCl (60 mL). The mixture was refluxed for 24 h. The mixture was concentrated to dryness then co-evaporated several time with methanol to give the desired 2-(3-methylamino-propylamino)-ethanol (399 mg, 2.46 mmol)
後処理
- temperatureThe mixture was refluxed for 24 hours under nitrogen
- temperatureto cool down
- concentrationThe reaction mixture was concentrated to low volume
- additiontreated with a 6M aqueous solution of HCl (60 mL)
- temperatureThe mixture was refluxed for 24 h
- concentrationThe mixture was concentrated to dryness
出典と根拠
- ORDレコード
- ord-c8e44cb9376444d0b77131b8e01d1a40
- 出典データセット
- uspto-grants-2012_06
- 特許番号
- US08202511B2
反応ノート
読み込み中…