反应详情

To a solution of 2.30 g (5.0 mmol) of 8-chlorodibenz[b,f][1,4]oxazepine-10(11H)-carboxylic acid, 2-[3-[[(1,1-dimethylethoxy)carbonyl]amino]-1-oxopropyl]hydrazide (7), prepared as described above in Example 7, in 8 mL of acetic acid (HOAc) was added 8 mL of 6.8 N HCl/dioxane. After 15 minutes, the solvent was removed under H2O aspirator vacuum. The resulting residue was triturated with diethyl ether (Et2O). The resulting white solid was collected on a sintered glass funnel and dried in a vacuum oven at 70° C. for 16 hours. A yield of 1.62 g (81%) of 8-chlorodibenz[b,f][1,4]oxazepine-10(11H)-carboxylic acid, 2-(3-amino-1-oxopropyl)hydrazide, monohydrochloride (9) was isolated. Analysis calculated for C17H17N4O3Cl.0.9 HCl.1.5 H2O: C, 48.54; H, 5.01; N, 13.32; Cl, 16.01. Found: C, 48.70; H, 4.77; N, 12.87; Cl, 16.07.

1. customthe solvent was removed under H2O
2. customThe resulting residue was triturated with diethyl ether (Et2O)
3. customThe resulting white solid was collected on a sintered glass funnel
4. customdried in a vacuum oven at 70° C. for 16 hours