Sodium Nitrite → rac-((1R,2S)-2-aminocyclohexyl)methanol
반응식
[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]참가 물질
4
반응 조건
- 온도
- 2.5 °C
실험 절차
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 oil.
후처리
- 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
출처 및 근거
- ORD 기록
- ord-6c1f1e15b3444fe194bfb3a8479f5e7c
- 출처 데이터셋
- uspto-grants-2001_03
- 특허 번호
- US06207862B1
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