反应详情

2,2,2-Trichloro-1,1-dimethylethyl chloroformate (2.77 g, 11.6 mmol) was added to a sol. of compound C4 (1.40 g, 2.31 mmol) in CH2ClCH2Cl (30 mL), and the mixture was heated to reflux for 2 h. 2,2,2-Trichloro-1,1-dimethylethyl chloroformate (1.40 g, 5.5 mmol) was added again, and the mixture was heated to reflux for 2 h. The mixture was allowed to cool to rt, and the solvents were removed under reduced pressure. The residue was diluted with EtOAc, and washed with aq. 1M NaOH (2×). The combined aq. layers were extracted back with EtOAc (2×). The combined org. extracts were dried over MgSO4, filtered, and the solvents were removed under reduced pressure. Purification of the residue by FC (EtOAc/heptane 1:4) yielded the title compound (815 mg, 44%). LC-MS: tR=1.25 min; ES+: 796.32.

1. temperaturethe mixture was heated
2. temperatureto reflux for 2 h
3. temperaturethe mixture was heated
4. temperatureto reflux for 2 h
5. customthe solvents were removed under reduced pressure
6. additionThe residue was diluted with EtOAc
7. washwashed with aq. 1M NaOH (2×)
8. extractionThe combined aq. layers were extracted back with EtOAc (2×)
9. dry with materialextracts were dried over MgSO4
10. filtrationfiltered
11. customthe solvents were removed under reduced pressure
12. customPurification of the residue by FC (EtOAc/heptane 1:4)