反应详情

温度

22 °C

A solution of the product from step g) (727 mg, 2.33 mmol) in anhydrous dichloroethane (11.6 ml) was cooled to 0° C., treated with 1-Chloroethyl chloroformate (1.27 ml, 11.65 mmol) and the reaction was warmed to 22° C. for 1 hour. The reaction diluted with CH2Cl2 (50 ml) and washed with sat. NaHCO3 (25 ml). The sat. NaHCO3 was back extracted with CH2Cl2 and the combined organic layers were washed with brine (25 ml), dried (MgSO4) and concentrated providing an oily residue, which was taken up in anhydrous MeOH (75 ml) and refluxed for 1 hour. The MeOH was evaporated and the crude residue was triturated with ether and filtered providing 323 mg (54%) of the subtitle compound. 1H NMR (300 MHz, DMSO) δ 9.60 (br s, 2H); 3.14-3.28 (m, 6H); 2.97-3.50 (m, 2H); MS: ESI (positive): 222, 224 (M+H).

1. washwashed with sat. NaHCO3 (25 ml)
2. extractionThe sat. NaHCO3 was back extracted with CH2Cl2
3. washthe combined organic layers were washed with brine (25 ml)
4. dry with materialdried (MgSO4)
5. concentrationconcentrated
6. customproviding an oily residue, which
7. temperaturerefluxed for 1 hour
8. customThe MeOH was evaporated
9. customthe crude residue was triturated with ether
10. filtrationfiltered