反应详情

The carboxylic acid from Example 154A (150 mg, 0.41 mmol) and 1-methyl-1-(3-trifluoromethyl-phenyl)ethylamine (Example 1A, 91.2 mg, 0.45 mmol) are placed in 4 ml DMF and treated at RT with 66.1 mg (0.49 mmol) of HOBt. After 10 mins, 101.6 mg (0.53 mmol) of EDC are added and the mixture stirred overnight at RT. It is then treated with water and ethyl acetate. The phases are separated, and the aqueous phase is extracted with ethyl acetate. The combined organic phases are washed with water, then with sat. sodium chloride solution, dried by filtration through an Extrelut cartridge and freed of the volatile components on the rotary evaporator. The residue is purified by chromatography on silica gel (Biotage cartridge 25M, eluent: cyclohexane/ethyl acetate 1:1). 192 mg (85% of theory) of the title compound are thus obtained.

1. customThe phases are separated
2. extractionthe aqueous phase is extracted with ethyl acetate
3. washThe combined organic phases are washed with water
4. dry with materialwith sat. sodium chloride solution, dried by filtration through an Extrelut cartridge
5. customfreed of the volatile components on the rotary evaporator
6. customThe residue is purified by chromatography on silica gel (Biotage cartridge 25M, eluent: cyclohexane/ethyl acetate 1:1)