反应详情

To a solution of (11-oxo-10,11-dihydro-5H-dibenzo[b,e][1,4]diazepin-2-yl)-thiourea (Example 9, 75 mg, 0.26 mmol) in ethanol (10 mL) was added chloroacetaldehyde (50% in water, 0.1 mL). The solution was refluxed for 5 hr and then concentrated under vacuum and poured into water (5 mL). The solution pH was adjusted to 9 with aqueous saturated sodium bicarbonate and then extracted with ethyl acetate. The organic phase was dried over magnesium sulfate and the solvent evaporated. The residue was recrystallized from ethanol/hexanes to give yellow solid (30 mg, 40%).

1. temperatureThe solution was refluxed for 5 hr
2. concentrationconcentrated under vacuum
3. additionpoured into water (5 mL)
4. extractionextracted with ethyl acetate
5. dry with materialThe organic phase was dried over magnesium sulfate
6. customthe solvent evaporated
7. customThe residue was recrystallized from ethanol/hexanes