反应详情

To an ice cold solution of 2 g of cis-[3-(methoxy-methyl-carbamoyl)-cyclobutyl]-acetic acid tert-butyl ester in 25 mL of dichloromethane was added 10 mL of trifluoroacetic acid. The mixture was allowed to warm and stir for 2 h then concentrated under reduced pressure. The residue was taken up in 3×50 mL of toluene and repeatedly concentrated under reduced pressure to remove trifluoroacetic acid. Drying under vacuum overnight gave 1.6 g of product as a colorless oil: MS (m+1)=202.3; 1H NMR (400 MHz, CDCl3) 9.0 (br s, 1H), 3.62 (s, 3H), 3.18 (s, 3H), 2.65 (m, 1H), 2.5 (overlapping d and m, 3H), 2.4 (dd, 1H), 2.0 (, m, 2H).

1. temperatureto warm
2. concentrationthen concentrated under reduced pressure
3. concentrationrepeatedly concentrated under reduced pressure
4. customto remove trifluoroacetic acid
5. customDrying under vacuum overnight