反应详情

A solution of 49 μl (0.39 mMol) phenyl chloroformiate in 1.5 ml THF is cooled to −70° C. Then a solution of 81 mg (0.33 mMol) 4-pyrrolidin-1-ylmethyl-3-trifluoromethyl-phenylamine and 0.3 ml pyridine in 1.5 ml THF is added dropwise. After 1 h, it is poured into a mixture of 20 g ice, 40 ml sat. Na2CO3/water 1:3 and 40 ml EtOAc. The aqueous layer is separated off and extracted 2× with EtOAc. The organic phases are washed with water and brine, dried (Na2SO4) and concentrated to the title compound: MS: [M+1]+=365; HPLC: AtRet=11.1.

1. customThe aqueous layer is separated off
2. extractionextracted 2× with EtOAc
3. washThe organic phases are washed with water and brine
4. dry with materialdried (Na2SO4)
5. concentrationconcentrated to the title compound