反应详情

温度

22 °C

A solution of the product from step (h) (assumed 0.35 mmol) in anhydrous dichloroethane (2 ml) was cooled to 0° C., treated with K2CO3 (˜50 mg) and 1-chloroethyl chloroformate (0.38 ml, 3.5 mmol). The reaction was allowed to warmed to 22° C. for 18 hours. The reaction diluted with CH2Cl2 (50 ml) and washed with sat. NaHCO3 (2×50 ml), brine (50 ml), dried (MgSO4) and solvent evaporated in vacuo providing an oily residue, which was dissolved in anhydrous MeOH (10 ml) and refluxed for 1.5 hours. The MeOH was evaporated in vacuo to give the crude product. A portion of the crude was purified by preparative HPLC-MS to give the title compound. 1H NMR (300 MHz, CDCl3) δ 6.25 (br s, 1 H); 3.05-3.19 (m, 8 H); 1.34 (s, 9 H); MS: ESI (positive): 272, 274 (M+H).

1. washwashed with sat. NaHCO3 (2×50 ml), brine (50 ml)
2. dry with materialdried (MgSO4) and solvent
3. customevaporated in vacuo
4. customproviding an oily residue, which
5. temperaturerefluxed for 1.5 hours
6. customThe MeOH was evaporated in vacuo
7. customto give the crude product
8. customA portion of the crude was purified by preparative HPLC-MS