反应详情

An ice cold mixture of 84 mg of 3-[N-(1-carboethoxy-3-phenylpropyl)amino]-5-methyl-1,3,4,5-tetrahydro-1,5-benzodiazepin-2-one, 15 mg of powdered potassium hydroxide and 6.5 mg of tetrabutylammonium bromide in 3 ml of dry tetrahydrofuran is treated with 32 mg of methyl bromoacetate. The reaction is allowed to stir for 3 hr at room temperature. At this time, the solution is filtered and concentrated and the residue dissolved in 20 ml of ethyl acetate. This is washed with 5 ml of water and dried over potassium carbonate. Concentration under reduced pressure affords 3-[N-(1-carboethoxy-3-phenylpropyl)amino]-1-carbomethoxymethyl-5-methyl-1,3,4,5-tetrahydro-1,5-benzo diazepin-2-one.

1. filtrationAt this time, the solution is filtered
2. concentrationconcentrated
3. dissolutionthe residue dissolved in 20 ml of ethyl acetate
4. washThis is washed with 5 ml of water
5. dry with materialdried over potassium carbonate
6. concentrationConcentration under reduced pressure