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Sodium Methoxide → HCID 54339002、化合物

HRID 477957
ノート
印刷プレビュー

反応式

HRID 477957 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 10942334Sodium MethoxideHCID 20144889HCID 20144889、化合物

生成物 1

HCID 54339002HCID 54339002、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

(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).

後処理

  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

出典と根拠

ORDレコード
ord-0674e0f4cf954d2391c1d7cbe947eaba
出典データセット
uspto-grants-1989_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04889848

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート