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Hydrogen chloride-ethyl acetate → 9-(Pyridin-4-yl)-2,3,4,5-tetrahydro-1,4-benzoxazepine dihydrochloride

HRID 886876
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인쇄 미리보기

반응식

HRID 886876 반응식
[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]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 21866389Hydrogen chloride-ethyl acetateHCID 68577733tert-butyl 9-(pyridin-4-yl)-2,3-dihydro-1,4-benzoxazepine-4(5H)-carboxylate

생성물 1

HCID 685785529-(Pyridin-4-yl)-2,3,4,5-tetrahydro-1,4-benzoxazepine dihydrochloride수율 19%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

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.

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후처리

  1. customthe solvent was evaporated under reduced pressure
  2. customThe residue was recrystallized from methanol

출처 및 근거

ORD 기록
ord-c238b60f29504fb7905728347146d18c
출처 데이터셋
uspto-grants-2012_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08247403B2

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