反应详情

To a cooled (0° C.) solution of 5-oxo-[1,4]diazepane-1-carboxylic acid tert-butyl ester 5.9 g (28 mmol) and 4-bromo-N-methoxy-N-methyl-butyramide 5.4 g (28 mmol) in DMF (220 ml) was added NaH 1.3 g (30 mmol, 55% dispersion in oil), the mixture allowed to reach RT and the mixture stirred for a further 2 h. The reaction was then concentrated, the residue redissolved in EtOAc and washed with 10% aq. KHSO4 solution, brine, dried (MgSO4) and concentrated affording the title compound 9.1 g (quant) as white foam. MS: 330.3 (MH+).

1. customto reach RT
2. concentrationThe reaction was then concentrated
3. dissolutionthe residue redissolved in EtOAc
4. washwashed with 10% aq. KHSO4 solution, brine
5. dry with materialdried (MgSO4)
6. concentrationconcentrated