反应详情

温度

25 °C

A solution of Example 4B (0.18 g, 0.6 mmol) in dichloromethane:trifluoroacetic acid (4 mL, 1:1) was stirred at 25° C. for 1 h, and the solvents were evaporated. This material was dissolved in THF (1 mL) and treated with diisopropylethyl amine (0.31 mL, 3 equivalents), DEPBT (0.36 g, 2 equivalents), and Example 18A (0.105 g, 1 equivalent), stirred at 25° C. for 3 h. The mixture was partitioned between dichloromethane and 10% sodium carbonate, the organic layer was separated, washed with brine, dried over sodium sulfate, filtered and the solvents were evaporated. The crude residue was purified using 2% methanol/chloroform to give 0.1 g (47%) of the title compound.

1. customthe solvents were evaporated
2. dissolutionThis material was dissolved in THF (1 mL)
3. customThe mixture was partitioned between dichloromethane and 10% sodium carbonate
4. customthe organic layer was separated
5. washwashed with brine
6. dry with materialdried over sodium sulfate
7. filtrationfiltered
8. customthe solvents were evaporated
9. customThe crude residue was purified