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Potassium Carbonate → 4,5-Diacetyl-[1,4,5]-oxadiazepine

HRID 1817778
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인쇄 미리보기

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HRID 1817778 반응식
[C:1]([NH:4][NH:5][C:6](=[O:8])[CH3:7])(=[O:3])[CH3:2].C(=O)([O-])[O-].[K+].[K+].[CH3:15][CH2:16][O:17][CH2:18][CH:19](Cl)Cl>CS(C)=O>[C:1]([N:4]1[N:5]([C:6](=[O:8])[CH3:7])[CH:19]=[CH:18][O:17][CH:16]=[CH:15]1)(=[O:3])[CH3:2]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 72884Acetic acid, 2-acetylhydrazideHCID 139875142,2-Dichlorodiethyl Ether

생성물 1

HCID 673358624,5-Diacetyl-[1,4,5]-oxadiazepine

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

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온도
20 °C

실험 절차

A mixture of 35 g of diacetylhydrazine (0.3 mol), 124.4 g or 165.8 g of ground potassium carbonate (0.9 or 1.2 mol, respectively), 85.8 g of 2,2-dichlorodiethyl ether (0.6 mol) and 560 ml of solvent (see Table 2) is heated to 125° C. and maintained at 125-130° C. or 80-90° C. (in the case of DMSO) for 5 hours. The mixture is then cooled to 20° C. and filtered, and the filtration residue is washed with the solvent. The yield is given by the content of title compound in the combined filtrate.

후처리

  1. filtrationfiltered
  2. washthe filtration residue is washed with the solvent

출처 및 근거

ORD 기록
ord-3eddec40a65242c0868f7faf96b798b2
출처 데이터셋
uspto-grants-2009_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07598376B2

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