反应详情

A solution of 2-methoxyethanamine (8.9 mL, 102.06 mmol) and chloride 75 (7.13 g, 34.02 mmol) in DMSO (20 mL) was heated at 60° C. 5 h. The mixture was then cooled to room temperature, diluted with EtOAc, washed with aqueous sodium bicarbonate, water and brine. The organic phase was further extracted with 1N HCl and the acid extract was collected and basified with 2N NaOH (pH˜11). The basic aqueous solution was extracted with DCM, the DCM extract was dried over anhydrous sodium sulphate, and concentrated under reduced pressure to afford title compound 76 (8.44 g, 99%) as brown foam. MS (m/z): 248.04 (M+H).

1. custom5 h
2. washwashed with aqueous sodium bicarbonate, water and brine
3. extractionThe organic phase was further extracted with 1N HCl
4. extractionthe acid extract
5. customwas collected
6. extractionThe basic aqueous solution was extracted with DCM
7. extractionthe DCM extract
8. dry with materialwas dried over anhydrous sodium sulphate
9. concentrationconcentrated under reduced pressure