反应详情

温度

0 °C

The 2-chloro-5,11-dihydro-11-ethyl-8-hydroxy-5-methyl-6H-dipyrido[3,2-b:2',3'-e][1,4]diazepin-6-one (0.052 g, 0.17 mmol) was dissolved in tetrahydrofuran and treated with excess sodium hydride (60% wt.) followed by benzyl bromide (0.04 mL, 0.34 mmol). After 24 hours stirring the mixture was cooled to 0° C. and the excess sodium hydride was quenched by the dropwise addition of water and the resulting solution was extracted with dichloromethane (3×20 mL) The combined organics were dried over magnesium sulfate, concentrated and the residue was purified by chromatography (hexanes to 1:1 hexanes/ethyl acetate gradient) followed by crystallization from hexanes to give the title compound (0.035 g, 52%), m.p. 159°-160° C.

1. customthe excess sodium hydride was quenched by the dropwise addition of water
2. extractionthe resulting solution was extracted with dichloromethane (3×20 mL) The combined
3. dry with materialorganics were dried over magnesium sulfate
4. concentrationconcentrated
5. customthe residue was purified by chromatography (hexanes to 1:1 hexanes/ethyl acetate gradient)
6. customfollowed by crystallization from hexanes