反应详情

A solution of the compound 98 (171.0 mg, 0.4 mmol) and 2-methoxyethanamine (0.14 mL, 1.62 mmol) in THF (98.1 mL) was stirred overnight at room temperature. It was then diluted with DCM, washed with aqueous sodium bicarbonate and water. The organic phase was extracted with 1N HCl, the aqueous acidic phase was basified by addition of 1N NaOH (pH˜11) and extracted with DCM. The DCM extract was dried over anhydrous sodium sulphate and concentrated under reduced pressure affording title compound 99 (89.0 mg, 45% yield) as cream foam. MS (m/z): 501.2 (M+1).

1. washwashed with aqueous sodium bicarbonate and water
2. extractionThe organic phase was extracted with 1N HCl
3. additionthe aqueous acidic phase was basified by addition of 1N NaOH (pH˜11)
4. extractionextracted with DCM
5. extractionThe DCM extract
6. dry with materialwas dried over anhydrous sodium sulphate
7. concentrationconcentrated under reduced pressure