Hydrogen chloride-ethyl acetate → 7-Phenyl-2,3,4,5-tetrahydro-1,4-benzoxazepine hydrochloride

HRID 886887노트

반응식

HRID 886887 반응식
[C:1]1([C:7]2[CH:8]=[CH:9][C:10]3[O:16][CH2:15][CH2:14][N:13](C(OC(C)(C)C)=O)[CH2:12][C:11]=3[CH:24]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C(OCC)(=O)C.[ClH:31]>C(OCC)(=O)C>[ClH:31].[C:1]1([C:7]2[CH:8]=[CH:9][C:10]3[O:16][CH2:15][CH2:14][NH:13][CH2:12][C:11]=3[CH:24]=2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

참가 물질

4

반응물 2

HCID 21866389Hydrogen chloride-ethyl acetateHCID 68578602tert-butyl 7-phenyl-2,3-dihydro-1,4-benzoxazepine-4(5H)-carboxylate

생성물 1

HCID 685797757-Phenyl-2,3,4,5-tetrahydro-1,4-benzoxazepine hydrochloride수율 91.1%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

A mixture of tert-butyl 7-phenyl-2,3-dihydro-1,4-benzoxazepine-4(5H)-carboxylate (160 mg, 0.471 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 a mixed solvent of methanol and ether to give the desired product (112 mg, 91.1%) as a solid.

후처리

  1. customthe solvent was evaporated under reduced pressure
  2. customThe residue was recrystallized from a mixed solvent of methanol and ether

출처 및 근거

ORD 기록
ord-24a9c3597fdc43128e34845c59f661c0
출처 데이터셋
uspto-grants-2012_08
특허 번호
US08247403B2

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