反应详情

5.2 ml of anhydrous triethylamine is added drop by drop to 5.3 g of product obtained in Stage B in 50 ml of methylene chloride. After cooling to 0°, +5° C., 3.5 ml of trimethylsilyl chloride in 15 ml of methylene chloride is introduced drop by drop, with agitation for 5 minutes at 0° C. and for 15 minutes at ambient temperature. The reaction mixture is poured into 200 ml of a water and ice mixture and 100 ml of isopropyl ether. After decanting, the organic phase is washed with water to obtain a pH of 7.5-8, and the aqueous phases with water are extracted by isopropyl ether. The organic phases are reunited, dried, concentrated to dryness and 6.81 g of expected product is obtained.

1. temperatureAfter cooling to 0°, +5° C.
2. waitfor 15 minutes at ambient temperature
3. customAfter decanting
4. washthe organic phase is washed with water
5. customto obtain a pH of 7.5-8
6. extractionthe aqueous phases with water are extracted by isopropyl ether
7. customdried
8. concentrationconcentrated to dryness