反应详情

Dissolve 1,4-dioxaspiro[4.5]decan-8-amine (785 mg, 0.005 mol; see Liebigs (1990) Ann. chem. 8:781-7) in CH2Cl2 and then add H2O (20 mL) followed by saturated NaHCO3 solution (50 mL). Add a toluene solution of phosgene (20% solution, 5 mL) to the reaction mixture and stir at room temperature for 1 hour. Dry the CH2Cl2 layer (Na2SO4) and concentrate under reduced pressure. Dissolve the resulting oil in dry toluene to produce a stock solution (˜0.2 M) of (1,4-dioxa-spiro[4.5]dec-8-yl)-carbamoyl chloride. B. 1′-(1,4-dioxa-spiro[4.5]dec-8-yl-carbamoyl)-spiro[isobenzofuran-1,4′-piperidin]-3-one

1. dry with materialDry the CH2Cl2 layer (Na2SO4)
2. concentrationconcentrate under reduced pressure
3. dissolutionDissolve the resulting oil in dry toluene