反应详情

To a -5° C. suspension of the nitrile from Step 6 (1.59 g, 3.88 mmol) in 15 mL methanol was added HCl gas to give a saturated solution. The mixture was then heated to reflux overnight, cooled and poured into ice water. The mixture was adjusted to pH 10 with 2.0N NaOH, and then extracted with ethyl acetate. The organic extracts were washed with saturated NaHCO3 and brine, dried over MgSO4 and evaporated. Purification by flash chromatography (15% ethyl acetate/hexanes) provided 1.63 g of the title compound.

1. customto give a saturated solution
2. temperatureThe mixture was then heated
3. temperatureto reflux overnight
4. temperaturecooled
5. extractionextracted with ethyl acetate
6. washThe organic extracts were washed with saturated NaHCO3 and brine
7. dry with materialdried over MgSO4
8. customevaporated
9. customPurification by flash chromatography (15% ethyl acetate/hexanes)