反应详情

A mixture of 0.3 g (0.00074 mole) of 6-(2-chlorophenyl)-1,8-dichloro-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxamide, 1.15 g (0.0028 mole) of sodium methoxide and 15 ml of methanol was heated at 120°-125° in a steel bomb for 24 hrs. The solvent was evaporated in vacuo. The residue was dissolved in methylene chloride, washed with water, dried and evaporated at reduced pressure to give a tan, amorphous solid. After chromatography over silica gel using 5% (v/v) of ethanol in methylene chloride the solid was recrystallized from a solution of ethanol and methylene chloride to give off-white crystals with mp 235°-238° (dec). Uv λ max 216 l mμ (ε=41,000) sh 243 (22,600) max 264 (20,000); ir (KBr) 3445, 3330, 3280 cm-1 (NH2) 1675 (CON) nmr (d-DMSO) δ 4.0 ppm (d, 1) and 5.88 (d, 1) (AB-system, J=12 Hz, C4 -H) 4.06 (s, 3, OCH3) 6.9-7.9 (m, 9, aromatic H and NH2).

1. customThe solvent was evaporated in vacuo
2. dissolutionThe residue was dissolved in methylene chloride
3. washwashed with water
4. customdried
5. customevaporated at reduced pressure
6. customto give a tan, amorphous solid
7. customAfter chromatography over silica gel using 5% (v/v) of ethanol in methylene chloride the solid was recrystallized from a solution of ethanol and methylene chloride
8. customto give off-white crystals with mp 235°-238° (dec)