反应详情

温度

40 °C

Methyl 2,3,4,5-tetrahydro-4-methyl-3-oxo-1H-1,4-benzodiazepine-2-acetate (100 g, 0.4 moles) was added to CH2Cl2 (500 ml) plus MeOH (500 ml) and heated at 40° C. for 0.5 hr. The solution was cooled to 26° C. and pyridine (64 g, 0.8 mole) added. Iodine monochloride (71.3 g, 0.44 mole) dissolved in CH2Cl2 (500 ml) was added dropwise over 30 minutes and the reaction stirred for a further 1.0 hr. The product was filtered off, washed with 60/80 petrol and dried in vacuo to yield the title compound (113 g, 75%).

1. temperatureThe solution was cooled to 26° C.
2. additionwas added dropwise over 30 minutes
3. filtrationThe product was filtered off
4. washwashed with 60/80 petrol
5. customdried in vacuo