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Acetic Acid → methyl 3-oxo-3,4-dihydro-2H-1,5-benzodioxepin-2-carboxylate

HRID 267787
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반응식

HRID 267787 반응식
[K].[O-]CCCC.[C:7]([CH2:11][O:12][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=1[O:19][CH2:20][C:21]([O:23][CH3:24])=[O:22])(OC)=[O:8].C(O)(=O)C>CS(C)=O.O>[O:8]=[C:7]1[CH2:11][O:12][C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=2[O:19][CH:20]1[C:21]([O:23][CH3:24])=[O:22]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 176Acetic AcidHCID 347859Methyl 2-methoxycarbonylmethyloxyphenoxyacetateHCID 5462222PotassiumHCID 12476378Butan-1-olate

생성물 1

HCID 13544514methyl 3-oxo-3,4-dihydro-2H-1,5-benzodioxepin-2-carboxylate

시약·촉매·용매 2

HCID 679Dimethyl Sulfoxide용매2회
HCID 962Water용매

실험 절차

Potassium t.-butoxide (15.8 g.) dissolved in DMSO (130 ml.) is added dropwise over a 45 minute period to 1,2-bis-carbomethoxymethoxybenzene (18.3 g.) in DMSO (30 ml.) under an atmosphere of nitrogen. The mixture then is stirred 3 hours at ambient temperature and a mixture of acetic acid (16 ml.) and water (200 ml.) is added. The reaction mixture is extracted with benzene, the powdery material removed by filtration and the benzene then dried over magnesium sulfate and the benzene then evaporated leaving 3-oxo-4-carbomethoxy-3,4-dihydro-2H-1,5-benzodioxepin that is used in the following step without purification.

후처리

  1. additionis added
  2. extractionThe reaction mixture is extracted with benzene
  3. customthe powdery material removed by filtration
  4. dry with materialthe benzene then dried over magnesium sulfate
  5. customthe benzene then evaporated

출처 및 근거

ORD 기록
ord-766110ea60d7478594a1f48108ef4b28
출처 데이터셋
uspto-grants-1976_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03944560

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