反应详情

To 0.65 g (1.61 mmol) of 3 dissolved in 20 mL of THF was added 6.4 mL (3.2 mmol) of a 0.5 M solution of 4-methylbenzylmagnesium chloride in THF via syringe over 10 min. After stirring at room temperature for 1 h, the reaction was quenched by addition of approximately 2 mL of saturated aqueous ammonium chloride. The reaction was then diluted with AcOEt and dried over sodium sulfate. Filtering the solution through a short plug of silica gel and concentrating in vacuo provided the crude product as an oil. Purification of this oil by flash chromatography eluting with 75% hexanes/AcOEt gave 0.64 g (89%) of the title compound as a white foam. MS Calcd.: 449. Found: 450 (M+H).

1. customthe reaction was quenched by addition of approximately 2 mL of saturated aqueous ammonium chloride
2. additionThe reaction was then diluted with AcOEt
3. dry with materialdried over sodium sulfate
4. filtrationFiltering the solution through a short plug of silica gel
5. concentrationconcentrating in vacuo
6. customprovided the crude product as an oil
7. customPurification of this oil by flash chromatography
8. washeluting with 75% hexanes/AcOEt