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Hydrochloric Acid → 7-acetyl-1-benzoxepin-3(2H)-one

HRID 1791039
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HRID 1791039 반응식
N12CCCN=C1CCCCC2.[C:12]([C:15]1[CH:16]=[CH:17][C:18]2[O:24][CH2:23][C:22](=[O:25])[CH2:21][CH:20](S(C3C=CC=CC=3)(=O)=O)[C:19]=2[CH:35]=1)(=[O:14])[CH3:13].O.Cl>ClCCl>[C:12]([C:15]1[CH:16]=[CH:17][C:18]2[O:24][CH2:23][C:22](=[O:25])[CH:21]=[CH:20][C:19]=2[CH:35]=1)(=[O:14])[CH3:13]
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참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 220422667-acetyl-5-(phenylsulfonyl)-4,5-dihydro-1-benzoxepin-3(2H)-one

생성물 1

HCID 220422637-acetyl-1-benzoxepin-3(2H)-one

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

0.084 ml (1.05 equivalents) of 1,8-diazabicyclo[5.4.0]undec-7-ene is added at ambient temperature, under nitrogen, to 184 mg (0.53 mmol) of 7-acetyl-5-(phenylsulfonyl)-4,5-dihydro-1-benzoxepin-3(2H)-one, prepared according to example 14, in suspension in 20 ml of dichloromethane. From the addition of the base, the medium becomes translucent and slightly yellow. After addition of water and 1N hydrochloric acid, the phases are separated by settling and then the aqueous phase is extracted three times with dichloromethane. The combined organic phases are washed with a saturated sodium hydrogencarbonate solution and then brine. After drying and then concentrating under vacuum, 90 mg (83%) of 7-acetyl-1-benzoxepin-3(2H)-one are obtained in the form of a white solid; M.p.=92–93° C.

후처리

  1. customprepared
  2. additionFrom the addition of the base
  3. customthe phases are separated
  4. extractionthe aqueous phase is extracted three times with dichloromethane
  5. washThe combined organic phases are washed with a saturated sodium hydrogencarbonate solution
  6. customAfter drying
  7. concentrationconcentrating under vacuum, 90 mg (83%) of 7-acetyl-1-benzoxepin-3(2H)-one
  8. customare obtained in the form of a white solid

출처 및 근거

ORD 기록
ord-4b1e0f16b5354988b0a789b4e223685d
출처 데이터셋
uspto-grants-2006_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07071340B2

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