反应详情

温度

0 °C

The compound obtained in step 1 (0.960 g, 1.69 mmol) was suspended in 9.6 ml of tert-butanol and cooled to 0° C. A solution of sodium dihydrogenphosphate (0.607 g, 5.06 mmol) in 2.4 ml or water, a 2 M solution of 2-methyl-but-2-ene in THF (5.06 ml, 10.11 mmol) and sodium chlorite (0.286 g, 2.53 mmol) were then added and the mixture was stirred for 3.75 h. Brine (30 ml) was added and the mixture was extracted three times with EA. The combined organic phases were washed twice with 1 N hydrochloric acid and once with brine, dried over sodium sulfate, filtered and evaporated to dryness. The residue was purified by chromatography on silica gel (DCM/MOH, 100:0, then 96:4) to give 0.398 g of the title compound.

1. extractionthe mixture was extracted three times with EA
2. washThe combined organic phases were washed twice with 1 N hydrochloric acid and once with brine
3. dry with materialdried over sodium sulfate
4. filtrationfiltered
5. customevaporated to dryness
6. customThe residue was purified by chromatography on silica gel (DCM/MOH, 100:0