反应详情

A solution of 0.339 g (1.03 mmol) of (S)-1-[4-(3-fluoro-benzyloxy)-phenyl]-5-oxo-pyrrolidine-3-carboxylic acid in 21 ml of N,N-dimethylformamide, cooled to 0° C., is treated consecutively with 0.15 ml (1.13 mmol) of triethylamine, 0.390 g (1.03 mmol) of HBTU, 0.085 g (1.24 mmol) of methylamine hydrochloride, and 0.15 ml (1.13 mmol) of triethylamine. The reaction is stopped after 30 min and the orange colored solution is evaporated under reduced pressure. The residue obtained is triturated in ethyl acetate, the white solid product is filtered, thereafter dissolved in dichloromethane and the solution washed three times with water. The organic phase is dried over sodium sulfate, then evaporated under reduced pressure to yield 231 mg (66% of theory) of a white solid. MS: m/e=343 (M+H)+; [α]589=−25.48° (c=0.954, CH2Cl2).

1. customthe orange colored solution is evaporated under reduced pressure
2. customThe residue obtained
3. customis triturated in ethyl acetate
4. filtrationthe white solid product is filtered
5. dissolutiondissolved in dichloromethane
6. washthe solution washed three times with water
7. dry with materialThe organic phase is dried over sodium sulfate
8. customevaporated under reduced pressure
9. customto yield 231 mg (66% of theory) of a white solid