反应详情

温度

70 °C

Add 0.6 ml of an 11.25N sodium hydroxide solution to a solution of 285 mg (0.68 mmol) of [1-({[5-(4-methoxyphenyl)-6-phenylfuro[2,3-d]pyrimidin-4-yl]oxy}methyl)cyclobutyl]methanol in 5 ml of toluene. After adding 23 mg (0.07 mmol) of tetra-n-butylammonium hydrogensulphate and 267 mg (1.37 mmol) of bromoacetic acid tert-butyl ester, stir the reaction mixture at 70° C. for20 h. After cooling to room temperature, adjust to pH 7 with conc. hydrochloric acid. Extract three times with 20 ml each time of dichloromethane. Wash the combined organic extracts with satd. aqueous sodium chloride solution, dry over sodium sulphate and filter. Concentrate the filtrate under reduced pressure. Purify the crude product by means of preparative RP-HPLC (gradient: water/acetonitrile). 260 mg (72% of theory) of the desired product are obtained.

1. temperatureAfter cooling to room temperature
2. extractionExtract three times with 20 ml each time of dichloromethane
3. washWash the combined organic extracts with satd
4. dry with materialaqueous sodium chloride solution, dry over sodium sulphate
5. filtrationfilter
6. concentrationConcentrate the filtrate under reduced pressure
7. customPurify the crude product by means of preparative RP-HPLC (gradient: water/acetonitrile)