反应详情

温度

75 °C

To (8-benzyl-10-vinyl-11-oxa-3,8-diazaspiro[5.5]undecan-3-yl)-(4-isopropoxy-3-methyl-phenyl)methanone (150 mg, 0.33 mmol), ammonium formate (74 mg, 1.17 mmol) and Pd (17 mg, 0.02 mmol) (10% on activated carbon) was added methanol (2 mL) and the reaction mixture was heated at 75° C. for 30 minutes. The reaction mixture was cooled, microfiltered and concentrated in vacuo, then diluted with DCM (20 mL), washed with aq. 1M NaOH (10 mL), extracted with DCM (120 mL), washed with brine (10 mL), dried over MgSO4 and concentrated in vacuo to give (10-ethyl-11-oxa-3,8-diazaspiro[5.5]undecan-3-yl)-(4-isopropoxy-3-methyl-phenyl)methanone (100 mg, 83%) as a colorless oil. ESI-MS m/z calc. 360.5. Found 361.3 (M+1)+; Retention time: 1.25 minutes (3 min run).

1. temperatureThe reaction mixture was cooled
2. concentrationmicrofiltered and concentrated in vacuo
3. additiondiluted with DCM (20 mL)
4. washwashed with aq. 1M NaOH (10 mL)
5. extractionextracted with DCM (120 mL)
6. washwashed with brine (10 mL)
7. dry with materialdried over MgSO4
8. concentrationconcentrated in vacuo