Sodium Nitrite → rac-((1R,2S)-2-aminocyclohexyl)methanol
反応式
[OH:1][CH2:2][C@@H:3]1[CH2:8][CH2:7][CH2:6][CH2:5][C@@H:4]1C(O)=O.[N:12]([O-])=O.[Na+]>OS(O)(=O)=O>[NH2:12][C@H:4]1[CH2:5][CH2:6][CH2:7][CH2:8][C@H:3]1[CH2:2][OH:1]参加物
4
反応条件
- 温度
- 2.5 °C
実験手順
The hydrazide of (1S,2R)-2-hydroxymethyl-1-cyclohexanecarboxylic acid (0.5 gram) is reacted with a solution of 0.5 grams of sodium nitrite in 10 ml of 5% H2SO4. The reaction mixture is maintained for 1 hour at 0-5° C, followed extraction of the reaction mixture with ethyl acetate, followed by basification of the resulting aqueous solution with NaOH, extraction with methyl t-butyl ether, drying of the extracts over MgSO4, filtration, and the removal of solvent by rotary evaporation. The product (1S,2R)-1-amino-2-(hydroxymethyl)cyclohexane is isolated as a light yellow
後処理
- extractionextraction of the reaction mixture with ethyl acetate
- extractionfollowed by basification of the resulting aqueous solution with NaOH, extraction with methyl t-butyl ether
- dry with materialdrying of the extracts over MgSO4, filtration
- customthe removal of solvent
- customby rotary evaporation
出典と根拠
- ORDレコード
- ord-67153227aa304517a461624e30a96b17
- 出典データセット
- uspto-grants-1999_06
- 特許番号
- US05916786
反応ノート
読み込み中…