反应详情

A solution of 15 g (0.066 mol) of 3,3-diphenylpropionic acid in 200 ml of acetic acid was treated with 2.25 g of platinum oxide and shaken on the Parr hydrogenator for 24 hours at a starting pressure of 60 lbs. Whenever the pressure dropped to approximately 45 lbs., the system was repressurized to 60 lbs. After heating on the steam bath to redissolve solid which had separated, the solution was decanted from the catalyst which had settled, filtered under argon, and the catalyst washed with additional acetic acid by decantation. The acetic acid was removed on a rotary evaporator to give a colorless solid (remaining acetic acid azeotroped with toluene). The solid was taken up in 250 ml of chloroform, filtered to clarify, and the chloroform evaporated. The product was suspended in ether and the evaporation repeated. After drying at reduced pressure for 2 hours, the solid weighed 15.25 g, melting point 118°-120° C. (s, 114° C.).

1. additionWhenever the pressure dropped to approximately 45 lbs
2. temperatureAfter heating on the steam bath
3. dissolutionto redissolve solid which
4. customhad separated
5. customthe solution was decanted from the catalyst which
6. filtrationfiltered under argon
7. washthe catalyst washed with additional acetic acid by decantation
8. customThe acetic acid was removed on a rotary evaporator
9. customto give
10. customa colorless solid (remaining acetic acid azeotroped with toluene)
11. filtrationfiltered
12. customthe chloroform evaporated
13. customthe evaporation
14. customAfter drying at reduced pressure for 2 hours
15. custom15.25 g, melting point 118°-120° C. (s, 114° C.)