反应详情

温度

75 °C

To (10-benzyl-8-phenyl-7-oxa-3,10-diazaspiro[5.5]undecan-3-yl)-(4-isopropoxy-3-methyl-phenyl)methanone (264 mg, 0.53 mmol), ammonium formate (167 mg, 2.65 mmol), palladium (30 mg, 0.03 mmol) (10% on carbon) was added methanol (5 mL) and the reaction mixture was stirred at 75° C. for 40 minutes. The reaction mixture was cooled, filtered over celite and concentrated in vacuo. The residue was partitioned between ethyl acetate and 1:1 sat. aq. NaHCO3/25% aq. NaOH, dried over MgSO4, filtered and concentrated in vacuo to give (4-isopropoxy-3-methyl-phenyl)-(8-phenyl-7-oxa-3,10-diazaspiro[5.5]undecan-3-yl)methanone (170 mg, 79%), which was used directly without further purification in the next step. ESI-MS m/z calc. 408.5. Found 409.7 (M+1)+; Retention time: 1.24 minutes (3 min run)

1. temperatureThe reaction mixture was cooled
2. filtrationfiltered over celite and
3. concentrationconcentrated in vacuo
4. customThe residue was partitioned between ethyl acetate and 1:1 sat. aq. NaHCO3/25% aq. NaOH
5. dry with materialdried over MgSO4
6. filtrationfiltered
7. concentrationconcentrated in vacuo