反应详情

温度

55 °C

To tert-butyl 4-[[benzyl-(2-hydroxy-2-phenyl-ethyl)amino]methyl]-4-hydroxy-piperidine-1-carboxylate (6.2 g, 14.07 mmol) was added HBr (60 mL of 48% w/w,) and the reaction mixture was stirred at 55° C. for 10 hours. The reaction mixture was evaporated in vacuo, basified the aqueous with 50% aq. NaOH to pH13, then extracted with DCM (3×75 mL). The combined organics were dried over MgSO4, filtered and concentrated in vacuo to give 4-benzyl-2-phenyl-1-oxa-4,9-diazaspiro[5.5]undecane (4.4 g, 97%) as a yellow oil, which was used directly without further purification. ESI-MS m/z calc. 322.2. found 323.7 (M+1)+; Retention time: 1.72 minutes (3 min run).

1. customThe reaction mixture was evaporated in vacuo
2. extractionextracted with DCM (3×75 mL)
3. dry with materialThe combined organics were dried over MgSO4
4. filtrationfiltered
5. concentrationconcentrated in vacuo