反应详情

To a solution of the amine from Preparation 2 (2 mmol, 350 mg) in 7 cm3 of anhydrous CH2Cl2 in the presence of Et3N (0.4 cm3 ; 1.5 eq.) is added, at 0° C., cyclobutylcarboxylic acid chloride (2 mmol; 0.24 cm3). Stirring is maintained for 1 h at room temperature and the medium is then washed twice with water. The organic phase is dried over MgSO4 and then evaporated. The residue is purified by chromatography on a column of silica gel (particle size 60-200 μm); eluent CH2Cl2 :MeOH 99:1. The expected compound is isolated and recrystallized from a CH2Cl2 :petroleum ether mixture to give 200 mg of the pure expected amide.

1. additionis added, at 0° C.
2. washthe medium is then washed twice with water
3. dry with materialThe organic phase is dried over MgSO4
4. customevaporated
5. customThe residue is purified by chromatography on a column of silica gel (particle size 60-200 μm)