反应详情

A solution of N-chlorosuccinimide (3.25 g, 24 mmol) in abs. DMF (18 ml) was added to a solution of compound V (2.7 g, 20 mmol) in abs. DMF (12 ml) at a temperature of 30-40° C. within 20 min. Cooling in an ice bath was carried out if necessary. The reaction mixture was stirred for 3 h at RT and then mixed with diethyl ether (175 ml) and water (115 ml). The phases were separated and the aqueous phase was extracted with diethyl ether (2×75 ml). The combined organic extracts were washed successively with water (100 ml) and sat. NaCl solution (100 ml). The organic phase was dried and concentrated. Compound W was obtained as a yellowish-green oil (3.33 g) and immediately reacted further.

1. temperatureCooling in an ice bath
2. customThe phases were separated
3. extractionthe aqueous phase was extracted with diethyl ether (2×75 ml)
4. washThe combined organic extracts were washed successively with water (100 ml) and sat. NaCl solution (100 ml)
5. customThe organic phase was dried
6. concentrationconcentrated