Hydrogen chloride-ethyl acetate → 9-Cyclopropyl-2,3,4,5-tetrahydro-1,4-benzoxazepine hydrochloride

HRID 886965노트

반응식

HRID 886965 반응식
[CH:1]1([C:4]2[C:14]3[O:13][CH2:12][CH2:11][N:10](C(OC(C)(C)C)=O)[CH2:9][C:8]=3[CH:7]=[CH:6][CH:5]=2)[CH2:3][CH2:2]1.C(OCC)(=O)C.[ClH:28]>C(OCC)(=O)C>[ClH:28].[CH:1]1([C:4]2[C:14]3[O:13][CH2:12][CH2:11][NH:10][CH2:9][C:8]=3[CH:7]=[CH:6][CH:5]=2)[CH2:3][CH2:2]1

참가 물질

4

반응물 2

HCID 21866389Hydrogen chloride-ethyl acetateHCID 68579262tert-butyl 9-cyclopropyl-2,3-dihydro-1,4-benzoxazepine-4(5H)-carboxylate

생성물 1

HCID 685789109-Cyclopropyl-2,3,4,5-tetrahydro-1,4-benzoxazepine hydrochloride수율 54%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

A mixture of tert-butyl 9-cyclopropyl-2,3-dihydro-1,4-benzoxazepine-4(5H)-carboxylate (70.0 mg, 0.242 mmol), ethyl acetate (1 ml) and 4N hydrogen chloride-ethyl acetate solution (2 ml) was stirred at room temperature for 1 hr, 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 (29.5 mg, 54.0%) 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-f3e64b57fc11497380f1e3f1427396ee
출처 데이터셋
uspto-grants-2012_08
특허 번호
US08247403B2

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