反应详情

6.4 ml of allyl chloroformate were added dropwise to 10.2 g of methanesulphonic acid (S)-1-benzyl-pyrrolidin-3-yl ester in 880 ml of n-heptane at room temperature within 10 minutes under argon and with slight cooling. The two-phase mixture was stirred vigorously for 2 hours 45 minutes and subsequently treated with 40 ml of methanol/water (1:1). The aqueous methanolic phase was separated, extracted with 40 ml of heptane and thereafter the methanol was distilled off on a rotary evaporator. The aqueous phase was extracted twice with 30 ml of ethyl acetate. The organic phases were combined, dried over Na2SO4, filtered and the filtrate was concentrated. 8.23 g of beige oil were obtained.

1. customThe aqueous methanolic phase was separated
2. extractionextracted with 40 ml of heptane
3. distillationthe methanol was distilled off on a rotary evaporator
4. extractionThe aqueous phase was extracted twice with 30 ml of ethyl acetate
5. dry with materialdried over Na2SO4
6. filtrationfiltered
7. concentrationthe filtrate was concentrated