反应详情

1-(3-Bromo-4-hydroxy-5-trifluoromethylphenyl)ethanone (6.8 g) was dissolved in absolute methanol (50 ml) and treated successively with DL-10-camphorsulfonic acid (111 mg) and trimethyl orthoformate (8 ml). After stirring at RT for 2 h, DMF (75 ml) and potassium carbonate (5.0 g) were added, followed by iodomethane (3 ml). After stirring for 6 h, the batch was allowed to stand overnight and was treated with a 1:1 mixture of n-heptane/water. After separating off the organic phase, it was additionally extracted once with n-heptane and then the combined heptane phases were dried over magnesium sulfate, filtered and concentrated. 7 g of the desired product were obtained.

1. stirringAfter stirring for 6 h
2. waitto stand overnight
3. customAfter separating off the organic phase, it
4. extractionwas additionally extracted once with n-heptane
5. dry with materialthe combined heptane phases were dried over magnesium sulfate
6. filtrationfiltered
7. concentrationconcentrated