Hydrogen chloride-ethyl acetate → HCID 68578308, compound
Reaction equation
[N:1]1([C:6]2[C:16]3[O:15][CH2:14][CH2:13][N:12](C(OC(C)(C)C)=O)[CH2:11][C:10]=3[CH:9]=[CH:8][CH:7]=2)[CH2:5][CH2:4][CH2:3][CH2:2]1.C(OCC)(=O)C.[ClH:30]>>[ClH:30].[ClH:30].[N:1]1([C:6]2[C:16]3[O:15][CH2:14][CH2:13][NH:12][CH2:11][C:10]=3[CH:9]=[CH:8][CH:7]=2)[CH2:5][CH2:4][CH2:3][CH2:2]1Participants
3
Procedure
A solution of tert-butyl 9-(pyrrolidin-1-yl)-2,3-dihydro-1,4-benzoxazepine-4(5H)-carboxylate (90.0 mg, 0.283 mmol) in 4N hydrogen chloride-ethyl acetate (3 ml) was stirred for 1 hr at room temperature, and the solvent was evaporated under reduced pressure. The residue was recrystallized from a mixed solvent of methanol and ether to give the desired product (25.4 mg, 30.9%) as a solid.
Workup
- customthe solvent was evaporated under reduced pressure
- customThe residue was recrystallized from a mixed solvent of methanol and ether
Sources & evidence
- ORD record
- ord-5da03bbad2b7415b8f0cf3510b4478d8
- Source dataset
- uspto-grants-2012_08
- Patent number
- US08247403B2
Reaction notes
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