反应详情

温度

70 °C

Add 0.5 ml of 11.25 N sodium hydroxide solution to a solution of 265 mg (0.62 mmol) 2-({[5-(4-ethylphenyl)-6-phenylfuro[2,3-d]pyrimidin-4-yl]oxy}methyl)-3,3-dimethylbutan-1-ol in 10 ml toluene. After adding 21 mg (0.06 mmol) tetra-n-butylammonium hydrogensulphate and 240 mg (1.23 mmol) 2-bromoacetic acid tert.-butyl ester, stir the reaction mixture for 16 h at 70° C. After cooling to room temperature, neutralize with 1 N hydrochloric acid and extract with ethyl acetate. Wash the organic phase with satd. aqueous sodium chloride solution, dry over sodium sulphate, and filter. Concentrate the filtrate by vacuum evaporation. Purify the residue by preparative RP-HPLC (gradient: water/acetonitrile). 170 mg (51% of theor.) of the desired product (racemate) is obtained.

1. temperatureAfter cooling to room temperature
2. extractionextract with ethyl acetate
3. washWash the organic phase with satd
4. dry with materialaqueous sodium chloride solution, dry over sodium sulphate
5. filtrationfilter
6. concentrationConcentrate the filtrate
7. customby vacuum evaporation
8. customPurify the residue by preparative RP-HPLC (gradient: water/acetonitrile)