Sodium Hydroxide → N-[4-(2-hydroxyethyl)phenyl]acetamide
反応式
C([O:4][CH2:5][CH2:6][C:7]1[CH:12]=[CH:11][C:10]([NH:13][C:14](=[O:16])[CH3:15])=[CH:9][CH:8]=1)(=O)C.[OH-].[Na+]>CO>[OH:4][CH2:5][CH2:6][C:7]1[CH:12]=[CH:11][C:10]([NH:13][C:14](=[O:16])[CH3:15])=[CH:9][CH:8]=1参加物
4
実験手順
A solution of the product from step (b) (55.3 g) in methanol (250 ml) and 1N aqu. NaOH (500 ml) was stirred at room temperature for 1 hour. The methanol was evaporated in vacuo and the remaining aqueous solution adjusted to pH 4 (2N aqu. HCl), saturated with NaCl, and extracted with ethyl acetate (×3). The combined extracts were washed with water and brine, dried over MgSO4 and evaporated in vacuo to give a brown oil which was flash chromatographed through a silica column using ethyl acetate and then crystallised from ethyl acetate to give the desired product (51.7 g).
後処理
- customThe methanol was evaporated in vacuo
- extractionextracted with ethyl acetate (×3)
- washThe combined extracts were washed with water and brine
- dry with materialdried over MgSO4
- customevaporated in vacuo
- customto give a brown oil which
- customchromatographed through a silica column
- customcrystallised from ethyl acetate
出典と根拠
- ORDレコード
- ord-1272854cfeea4a5086343221f74d5334
- 出典データセット
- uspto-grants-1993_07
- 特許番号
- US05225431
反応ノート
読み込み中…