反应详情

A solution consisting of 5-Benzyloxy-2-(4-benzyloxy-phenyl)-3-methyl-1H-indole No. 7 (6.5 g, 15.5 mmol) in DMF (60 mL) was cooled to 0° C. and treated with addition of sodium hydride (0.68 g, 17.0 mmol) and stirred for 20 minutes. A solution of 4-(3-chloropropoxy)-benzyl bromide No. 163 in DMF (10 mL) was then added slowly. The reaction was allowed to come to rt and stirred for 2 hours. The reaction was poured into water and extracted with ethyl acetate. The ethyl acetate was washed with water, brine and dried over magnesium sulfate and concentrate. The concentrate was treated with methanol and 5 g of the desired product precipitated as a white solid with a melting point of 130-132° C.

1. customto come to rt
2. stirringstirred for 2 hours
3. extractionextracted with ethyl acetate
4. washThe ethyl acetate was washed with water, brine
5. dry with materialdried over magnesium sulfate
6. concentrationconcentrate
7. additionThe concentrate was treated with methanol and 5 g of the desired product
8. customprecipitated as a white solid with a melting point of 130-132° C.