反应详情

To a solution of 6c (104 mg, 0.21 mmol) and triethylamine (0.1 mL, 3.3 eq) in 1 mL of DCM, was added isopropyl chloroformate (0.24 mL, 1.1 eq). The mixture was stirred at room temperature for 2 h. The crude mixture was poured onto silica and eluted with ethyl acetate/hexane then chromatographed over a silica gel column (elution with 25-100% ethyl acetate and 0.1% TEA in hexanes) and finally purified on preparative HPLC to give 6-1, LC-MS 460.4 (MH+), tR=4.50 (Method 4). EC50: 611 nM.

1. washeluted with ethyl acetate/hexane
2. customthen chromatographed over a silica gel column (elution with 25-100% ethyl acetate and 0.1% TEA in hexanes)
3. customfinally purified on preparative HPLC
4. customto give 6-1, LC-MS 460.4 (MH+), tR=4.50 (Method 4)