反应详情

In a reaction vessel, 100 mg of methyl (S)-2-amino-4,4-difluoropentanoate hydrochloride (0.49 mmol) were admixed with 320 mg of N,O-bis(trimethylsilyl)-acetamide (3.2 eq.) in 3 ml of acetonitrile. The reaction mixture was treated at 100° C. in a microwave for 30 min. 128 mg of 8-azaspiro[4.5]decane-8-sulfonyl chloride (1.1 eq.), dissolved in 2.5 ml of acetonitrile, were then added and the resulting reaction mixture was treated at 100° C. in a microwave for a further 2.5 h. The reaction mixture was concentrated under reduced pressure and the resulting residue was purified by preparative HPLC (gradient: acetonitrile/water and addition of 0.05% TFA). Methyl (S)-2-(8-azaspiro[4.5]decane-8-sulfonylamino)-4,4-difluoropentanoate was obtained as a colorless amorphous material.

1. additionThe reaction mixture was treated at 100° C. in a microwave for 30 min
2. additionwere then added
3. customthe resulting reaction mixture
4. additionwas treated at 100° C. in a microwave for a further 2.5 h
5. concentrationThe reaction mixture was concentrated under reduced pressure
6. customthe resulting residue was purified by preparative HPLC (gradient: acetonitrile/water and addition of 0.05% TFA)