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Sodium Methoxide → HCID 54339002, 화합물

HRID 477957
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HRID 477957 반응식
[S:1]1[C:7]2[C:8](=[C:11](C(OCC)=O)[C:12]([O:14][CH2:15][CH3:16])=[O:13])[CH2:9][S:10][C:6]=2[CH2:5][NH:4][CH2:3][CH2:2]1.C[O-].[Na+]>C(O)C>[S:1]1[C:7]2[C:8](=[CH:11][C:12]([O:14][CH2:15][CH3:16])=[O:13])[CH2:9][S:10][C:6]=2[CH2:5][N:4]=[CH:3][CH2:2]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 10942334Sodium MethoxideHCID 20144889HCID 20144889, 화합물

생성물 1

HCID 54339002HCID 54339002, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

(cb) 2.56 g of diethyl [3,4-dihydrothieno[2,3-f][1,4]thiazepin-8(5H)-ylidene]malonate was suspended in 15.6 ml of ethanol and, after the addition of 4.3 ml of 2N ethanolic sodium methylate solution, the mixture was heated to reflux until the reaction was completed. The solvent was removed in vacuo and the residue was taken up in 60 ml of water and extracted several times with methylene chloride. After washing the organic phases with water and drying with sodium sulfate, they were chromatographed on silica gel. After recrystallization, there was obtained ethyl [6,7-dihydrothieno[2,3-f][1,4]thiazepine-8-(5H)-ylidene]acetate in the form of yellowish crystals, m.p. 86°-87° (ethanol).

후처리

  1. temperaturethe mixture was heated
  2. temperatureto reflux until the reaction
  3. customThe solvent was removed in vacuo
  4. extractionextracted several times with methylene chloride
  5. washAfter washing the organic phases with water
  6. dry with materialdrying with sodium sulfate, they
  7. customwere chromatographed on silica gel
  8. customAfter recrystallization

출처 및 근거

ORD 기록
ord-0674e0f4cf954d2391c1d7cbe947eaba
출처 데이터셋
uspto-grants-1989_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04889848

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