反应详情

To a solution of 34-1 (72.5 mg, 0.18 mmol) and triethylamine (0.15 mL, 1.07 mmol) in 1 mL of DCM, was added mercury chloride (60 mg, 0.22 mmol) and di-Boc-thiourea (60 mg, 0.22 mmol). The mixture was stirred at room temperature for 4 h. It was then diluted with DCM (40 mL), filtered through a pad of celite, water (40 mL) was added to the filtrate and the layers were separated. The aqueous layer was extracted with DCM (2×40 mL), the combined extracts were dried over magnesium sulfate, filtered and the solvent was removed under vacuum to give a yellow oil. The oil was dissolved in DCM (5 mL) and TFA (2 mL, 25.96 mmol) was added. The mixture was stirred at room temperature for 1 h and then concentrated and dissolved in DCM for purification on preparative HPLC to give 36-1: LC-MS 453.1 (MH), tR=5.05 (Method 2). EC50: 1320 nM.

1. filtrationfiltered through a pad of celite, water (40 mL)
2. additionwas added to the filtrate
3. customthe layers were separated
4. extractionThe aqueous layer was extracted with DCM (2×40 mL)
5. dry with materialthe combined extracts were dried over magnesium sulfate
6. filtrationfiltered
7. customthe solvent was removed under vacuum
8. customto give a yellow oil
9. stirringThe mixture was stirred at room temperature for 1 h
10. concentrationconcentrated
11. dissolutiondissolved in DCM for purification on preparative HPLC
12. customto give 36-1