反应详情

温度

0 °C

Mercuric chloride (41 mg, 0.15 mmol) was added to a mixture of 6-phenethyl-7-(trifluoromethyl)-1,2,3,4-tetrahydro-[1,4]diazepino[6,7,1-hi]indole (prepared as described in Example 2 above, 53 mg, 0.14 mmol), bis-N-Boc thiourea (38 mg, 0.14 mmol) and triethylamine (0.45 mmol) in DMF (5 mL) at 0° C. After 1 h of stirring at 0° C., ethyl acetate was added. The resulting mixture filtered and the filtrate washed sequentially with water and brine then dried (Na2SO4) and concentrated. The resulting residue was purified by reverse-phase chromatography to yield Z-tert-butyl(((tert-butoxycarbonyl)imino)(6-phenethyl-7-(trifluoromethyl)-3,4-dihydro-[1,4]diazepino[6,7,1-hi]indol-2(1H)-yl)methyl)carbamate (74 mg, MS m/z=587 (MH+).

1. filtrationThe resulting mixture filtered
2. washthe filtrate washed sequentially with water and brine
3. dry with materialthen dried (Na2SO4)
4. concentrationconcentrated
5. customThe resulting residue was purified by reverse-phase chromatography