反应详情

A solution of D3 (500 mg) and benzoyl chloride (0.6 ml; 5.12 mmol) in pyridine (15 ml) is stirred at RT for 20 h. After completion, water is added and the aqueous layer is extracted with EtOAc. The combined organic layer is washed with hydrochloric acid (1 N), saturated NaHCO3 solution and brine, dried over Na2SO4 and concentrated in vacuo. Purification by flash chromatography on silica gel eluting with CH2Cl2/MeOH (30:1) afford the title compound (484 mg).

1. extractionthe aqueous layer is extracted with EtOAc
2. washThe combined organic layer is washed with hydrochloric acid (1 N), saturated NaHCO3 solution and brine
3. dry with materialdried over Na2SO4
4. concentrationconcentrated in vacuo
5. customPurification by flash chromatography on silica gel eluting with CH2Cl2/MeOH (30:1)