反应详情

To a solution of 2-[4-(tert-butoxycarbonylamino)cyclohexyl]acetic acid (1.0 g, 4 mmol) in DMF (10 mL) was added K2CO3 (600 mg, 4 mmol) followed by benzyl bromide (0.5 mL, 4.2 mmol). The resulting mixture was stirred for 16.75 hours, diluted with ether, washed with water (2×) followed by brine, dried over magnesium sulfate and concentrated. The residue was taken up in dichloromethane (12 mL). To this solution was added TFA (3 mL). The resulting solution was stirred for 2.5 hours then concentrated under reduced pressure. The residue was taken up in ethyl acetate, washed with saturated sodium bicarbonate solution followed by brine, dried over magnesium sulfate and concentrated under reduced pressure to give the title compound as a white solid.

1. washwashed with water (2×)
2. dry with materialdried over magnesium sulfate
3. concentrationconcentrated
4. additionTo this solution was added TFA (3 mL)
5. stirringThe resulting solution was stirred for 2.5 hours
6. concentrationthen concentrated under reduced pressure
7. washwashed with saturated sodium bicarbonate solution
8. dry with materialdried over magnesium sulfate
9. concentrationconcentrated under reduced pressure