反应详情

A solution of methanesulfonyl chloride (33 mg, 0.3 mmol) in dichloromethane (4 ml) was treated with a solution of Example 3 (103 mg, 0.3 mmol) in methanol (1 ml). The mixture was stirred at room temperature for 2 hours then diluted with dichloromethane and sodium hydrogen carbonate solution. The aqueous layer was then separated and extracted with additional dichloromethane. The combined organic layers were then washed with brine, dried over anhydrous magnesium sulphate, filtered and concentrated at reduced pressure. The residue was chromatographed on silica gel eluting with dichloromethane/methanol/0.880 ammonia solution (10:1:0.1) to give the title compound (16 mg, 13%) as a pale yellow solid; MS(ES+) m/e 421/423 [M+H]+.

1. customThe aqueous layer was then separated
2. extractionextracted with additional dichloromethane
3. washThe combined organic layers were then washed with brine
4. dry with materialdried over anhydrous magnesium sulphate
5. filtrationfiltered
6. concentrationconcentrated at reduced pressure
7. customThe residue was chromatographed on silica gel eluting with dichloromethane/methanol/0.880 ammonia solution (10:1:0.1)