反应详情

温度

0 °C

To a stirring solution of 3-[(2-chloro-3-trifluoromethyl-benzyl)-(2,2-diphenyl-ethyl)-amino]-propan-1-ol (448 mg, 1.0 mmol) in toluene (30 mL) was added 4-(3-hydroxy-phenyl)-piperazine-1-carboxylic acid tert-butyl ester (419 mg, 1.50 mmol). Polymer bound triphenylphosphine (500 mg, 1.50 mmol, 3 mmol/g, Fluka Chemie) was then added, and the mixture stirred for 15 minutes. The reaction mixture was then cooled to 0° C. and diisopropylazodicarboxylate (303 mg, 1.50 mmol) was added in a dropwise fashion. After stirring at room temperature overnight, the crude reaction mixture was filtered and the solid washed with toluene. Concentration of the filtrate in vacuo followed by purification by flash silica gel chromatography (silica gel 60, EM science; 15% EtOAc:hexane) afforded title compound as an oil (0.59 g, 84%). MS(ES) m/e 708.4 (M+).

1. additionwas then added
2. stirringAfter stirring at room temperature overnight
3. customthe crude reaction mixture
4. filtrationwas filtered
5. washthe solid washed with toluene
6. customConcentration of the filtrate in vacuo followed by purification by flash silica gel chromatography (silica gel 60, EM science; 15% EtOAc:hexane)