Hydrogen chloride-ethyl acetate → 9-(Pyridin-4-yl)-2,3,4,5-tetrahydro-1,4-benzoxazepine dihydrochloride
Reaction equation
[N:1]1[CH:6]=[CH:5][C:4]([C:7]2[C:17]3[O:16][CH2:15][CH2:14][N:13](C(OC(C)(C)C)=O)[CH2:12][C:11]=3[CH:10]=[CH:9][CH:8]=2)=[CH:3][CH:2]=1.C(OCC)(=O)C.[ClH:31]>C(OCC)(=O)C>[ClH:31].[ClH:31].[N:1]1[CH:2]=[CH:3][C:4]([C:7]2[C:17]3[O:16][CH2:15][CH2:14][NH:13][CH2:12][C:11]=3[CH:10]=[CH:9][CH:8]=2)=[CH:5][CH:6]=1Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
A mixture of tert-butyl 9-(pyridin-4-yl)-2,3-dihydro-1,4-benzoxazepine-4(5H)-carboxylate (109 mg, 0.334 mmol), ethyl acetate (1 ml) and 4N hydrogen chloride-ethyl acetate solution (4 ml) was stirred for 1 hr at room temperature, and the solvent was evaporated under reduced pressure. The residue was recrystallized from methanol to give the desired product (19.0 mg, 19.0%) as a solid.