反应详情

温度

90 °C

Methyl 3-(tert-butyldimethylsilyloxy)-2,2-dimethylpropanoate (0.63 g, 2.557 mmol) was added to toluene and NaH (0.4090 g, 10.23 mmol) and acetonitrile (0.534 mL, 10.23 mmol) and stirred overnight in a sealed vessel for 6 hours at 90° C. The solids were removed by filtration and rinsed with toluene. The toluene filtrate was concentrated, and the resulting solids were added to 3 N HCl, stirred for 30 minutes and then washed with ether. The mixture was concentrated and the resulting solids were rinsed several times with DCM. The DCM was dried over MgSO4, filtered and evaporated to provide the title compound as an oil (320 mg), which was used directly in the next step.

1. customThe solids were removed by filtration
2. washrinsed with toluene
3. concentrationThe toluene filtrate was concentrated
4. additionthe resulting solids were added to 3 N HCl
5. stirringstirred for 30 minutes
6. washwashed with ether
7. concentrationThe mixture was concentrated
8. washthe resulting solids were rinsed several times with DCM
9. dry with materialThe DCM was dried over MgSO4
10. filtrationfiltered
11. customevaporated