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Diethyl (ethoxymethylene)malonate → HCID 178469815, 화합물

HRID 570006
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반응식

HRID 570006 반응식
[OH-].[Na+].S(O)(O)(=O)=O.[C:8]([N:11]1[CH2:16][CH2:15][N:14]([CH2:17][C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[CH2:13][CH2:12]1)(=[NH:10])[NH2:9].C([O:26][CH:27]=[C:28]([C:34](OCC)=O)[C:29]([O:31][CH2:32][CH3:33])=[O:30])C>C(O)C>[CH2:17]([N:14]1[CH2:15][CH2:16][N:11]([C:8]2[N:9]=[C:27]([OH:26])[C:28]([C:29]([O:31][CH2:32][CH3:33])=[O:30])=[CH:34][N:10]=2)[CH2:12][CH2:13]1)[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6871Diethyl (ethoxymethylene)malonateHCID 14798Sodium HydroxideHCID 27566524-Benzylpiperazine-1-carboxamidine hemisulfate

생성물 1

HCID 178469815HCID 178469815, 화합물수율 64%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

An ethanol solution of 25.2 g of sodium hydroxide was added with 160 g (0.60 mol) of 1-amidino-4-benzylpiperazine sulfate, followed by a dropwise addition of 129.4 g (0.60 mol) of diethyl ethoxymethylenemalonate over 20 minutes. After being refluxed for 5.5 hours, the reaction mixture was cooled and the precipitated crystals were collected by filtration. The thus-obtained crystals were washed with water and then dried, thereby obtaining 131.4 g of the above-identified compound (yield: 64%).

후처리

  1. temperatureAfter being refluxed for 5.5 hours
  2. temperaturethe reaction mixture was cooled
  3. filtrationthe precipitated crystals were collected by filtration
  4. washThe thus-obtained crystals were washed with water
  5. customdried

출처 및 근거

ORD 기록
ord-4f8d268c255d4bcc9493bf3ff2360d98
출처 데이터셋
uspto-grants-1988_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04734418

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