反应详情

Trans-2-Aminocyclohexanecarboxylic acid (0.150 g, 1.05 mmol) is dissolved in 1.5 ml of water and NaOH (0.09 g, 2.25 mmol) in 1.5 ml of water is added at 0° C. 4-Chlorobenzene sulfonyl chloride (0.243 g, 1.15 mmol) in 1.5 ml of toluene is added. The reaction mixture is stirred at room temperature for 16 hours. The toluene layer is separated and the aqueous layer is washed twice with toluene. The toluene layers are discarded. Ethyl acetate is added to the aqueous layer (15 ml) and 2M HCl until pH<7. The two phases are separated and the aqueous layer is extracted with ethyl acetate (3×15 mL). The combined organic phases are washed with brine (20 ml), dried over MgSO4 and the ethyl acetate is removed under reduced pressure leaving a white solid that is dissolved in toluene (2×10 ml) and concentrated .The product is dried in vacuum.

1. customThe toluene layer is separated
2. washthe aqueous layer is washed twice with toluene
3. additionEthyl acetate is added to the aqueous layer (15 ml) and 2M HCl until pH<7
4. customThe two phases are separated
5. extractionthe aqueous layer is extracted with ethyl acetate (3×15 mL)
6. washThe combined organic phases are washed with brine (20 ml)
7. dry with materialdried over MgSO4
8. customthe ethyl acetate is removed under reduced pressure
9. customleaving a white solid
10. concentrationconcentrated .The product
11. customis dried in vacuum