反应详情

5.91 Grams (50 mmol) of methyl 3-hydroxybutyrate and 3.74 g (55 mmol) of imidazole were dissolved in 20 ml of DMF and thereto 8.29 g (55 mmol) of t-butyldimethylsilylchloride was added in several portions. After stirring the mixture at room temperature for 30 minutes, ice water was added and extraction with diethyl ether was conducted three times. The extract was washed with a saturated solution of NaCl, dried with anhydrous magnesium sulfate and concentrated under reduced pressure. The concentrate was distilled (62° to 68° C./5 mmHg) to give 10.51 g of methyl (-)-3-t-butyldimethylsilyloxybutyrate (yield: 91%).

1. extractionextraction with diethyl ether
2. washThe extract was washed with a saturated solution of NaCl
3. dry with materialdried with anhydrous magnesium sulfate
4. concentrationconcentrated under reduced pressure
5. distillationThe concentrate was distilled (62° to 68° C./5 mmHg)