反应详情

温度

0 °C

3-tert-Butyl-N-methoxy-N-methyl-5-[3-(tetrahydropyran-2-yloxy)propoxy]benzamide (O3.059; 5.49 g) was dissolved in THF (100 ml), cooled to 0° C. and admixed with lithium bis(trimethylsilyl)amide (14.47 ml, 1 M in MTB ether). After stirring at 0° C. for 30 min, methylmagnesium bromide (9.65 ml, 3 M in ether) was added dropwise. The cooling bath was removed and, after stirring at RT for 2 h, the mixture was diluted with water and extracted by shaking with EA. The EA phase was dried over magnesium sulfate, filtered and concentrated by rotary evaporation. The residue was purified using silica gel (200 g, n-heptane/EA 4:1). 3.4 g of the title compound were obtained.

1. customThe cooling bath was removed
2. stirringafter stirring at RT for 2 h
3. additionthe mixture was diluted with water
4. extractionextracted
5. stirringby shaking with EA
6. dry with materialThe EA phase was dried over magnesium sulfate
7. filtrationfiltered
8. concentrationconcentrated by rotary evaporation
9. customThe residue was purified