反应详情

A solution of 60.0 mmol of (1-amino-5-methoxyindan-1-yl)methanol in 120 ml of acetonitrile and 40 ml of methanol is cooled to −10° C. and 69 mmol of triethylamine and, dropwise over the course of 1 hour, 80.5 mmol of chloroacetyl chloride are successively added. The reaction mixture is warmed to room temperature and stirred for 3 hours. The reaction mixture is poured into water and extracted with tert-butyl methyl ether. The combined organic phases are washed with brine, dried with sodium sulphate and evaporated. The title compound is obtained as a beige solid which is employed without further purification for the next stage. Rf=0.15 (ethyl acetate-heptane 1:1); Rt=3.01 (gradient I).

1. extractionextracted with tert-butyl methyl ether
2. washThe combined organic phases are washed with brine
3. dry with materialdried with sodium sulphate
4. customevaporated