反应详情

A solution of 0.050 g (0.16 mmol) of (S)-1-[4-((S)-4-hydroxy-6-aza-spiro[2.5]oct-6-yl)-4-oxo-butyl]-3-methyl-piperazin-2-one (intermediate 13) and 0.053 ml (0.48 mmol) of 4-methylmorpholine in 1 ml of dichloromethane was treated at RT with 0.033 g (0.16 mmol) of 1-isocyanato-4-trifluoromethoxy-benzene (intermediate 14) in 1 ml of dichloromethane. After 1 h again 0.005 g of 0.033 g (0.16 mmol) of 1-isocyanato-4-trifluoromethoxy-benzene (intermediate 14) were added and after 30 min the reaction was extracted with aqueous 10% KHSO4/EtOAc (3×). The organic phases were washed with aqueous saturated NaHCO3, 10% NaCl and dried over Na2SO4 to yield, after precipitation with dichloromethane/pentane, 0.077 g (93%) of the titled compound as white amorphous solid. MS: 513.23 (MH+).

1. extractionwas extracted with aqueous 10% KHSO4/EtOAc (3×)
2. washThe organic phases were washed with aqueous saturated NaHCO3, 10% NaCl
3. dry with materialdried over Na2SO4
4. customto yield
5. customafter precipitation with dichloromethane/pentane, 0.077 g (93%) of the titled compound as white amorphous solid