反应详情

温度

65 °C

A mixture of 9-tert-butyl 2-methyl 4-benzyl-1-oxa-4,9-diazaspiro[5.5]undecane-2,9-dicarboxylate (670 mg, 1.66 mmol), ammonium formate (623 mg, 9.936 mmol) and palladium, 10 wt. % on activated carbon (353 mg, 3.31 mmol) in EtOH (5 mL) was heated at 65° C. for 50 minutes. The reaction mixture was cooled to room temperature, filtered and partitioned between EtOAc/1M aq. NaOH. The layers were separated and the organic layer was dried over Na2SO4, filtered and concentrated in vacuo to yield 9-tert-butyl 2-methyl 1-oxa-4,9-diazaspiro[5.5]undecane-2,9-dicarboxylate as a foam (386 mg, 74%). ESI-MS m/z calc. 314.2. found 315.5 (M+1)+; Retention time: 0.99 minutes (3 min run).

1. temperatureThe reaction mixture was cooled to room temperature
2. filtrationfiltered
3. custompartitioned between EtOAc/1M aq. NaOH
4. customThe layers were separated
5. dry with materialthe organic layer was dried over Na2SO4
6. filtrationfiltered
7. concentrationconcentrated in vacuo