反应详情

Add 2.2 ml of 45% sodium hydroxide solution to a mixture of 900 mg (2.31 mmol) 3-{[5-(4-methoxyphenyl)-6-phenylfuro[2,3-d]pyrimidin-4-yl]oxy}butan-2-ol, 1477 mg (11.53 mmol) tert.-butyl acrylate and 157 mg (0.46 mmol) tetra-n-butylammonium hydrogensulphate in 10 ml dichloromethane at 0° C., and stir at this temperature for one hour. After a further 16 hours at room temperature, filter the reaction mixture, and concentrate the filtrate by vacuum evaporation. Purify the raw product by preparative RP-HPLC (gradient: water/acetonitrile). 690 mg (57% of theor.) of the desired product is obtained as (R,S/S,R) racemate.

1. waitAfter a further 16 hours at room temperature
2. filtrationfilter the reaction mixture
3. concentrationconcentrate the filtrate
4. customby vacuum evaporation
5. customPurify the raw product by preparative RP-HPLC (gradient: water/acetonitrile)