反应详情

To a solution of tert-butyl 8-[(4-methoxyphenyl)methyl]-9-phenyl-11-oxa-3,8-diazaspiro[5.5]undecane-3-carboxylate (500 mg, 1.11 mmol) in DCM (1 mL) was added HCl (3 mL of 4 M in dioxane, 11.05 mmol) dropwise. The reaction mixture was stirred overnight at room temperature. The solvent was concentrated in vacuo and the residue was dissolved in the minimum amount of DCM and precipitated with ether. The solvent was decanted and the residue was again washed with ether and dried to give 8-[(4-methoxyphenyl)methyl]-9-phenyl-11-oxa-3,8-diazaspiro[5.5]undecane (400 mg, 93%). ESI-MS m/z calc. 352.2. found 353.7 (M+1)+; Retention time: 0.99 minutes (3 min run).

1. concentrationThe solvent was concentrated in vacuo
2. dissolutionthe residue was dissolved in the minimum amount of DCM
3. customprecipitated with ether
4. customThe solvent was decanted
5. washthe residue was again washed with ether
6. customdried