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HCID 241612、化合物 → HCID 13476441、化合物

HRID 1981870
ノート
印刷プレビュー

反応式

HRID 1981870 の反応式
[C:1]([CH:9]=[CH:10][C:11]([O:13][CH3:14])=[O:12])(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:15]([OH:18])(=[S:17])[CH3:16]>C(OCC)C>[C:15]([S:17][CH:10]([CH2:9][C:1](=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1)[C:11]([O:13][CH3:14])=[O:12])(=[O:18])[CH3:16]
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 241612HCID 241612、化合物HCID 178418634HCID 178418634、化合物

生成物 1

HCID 13476441HCID 13476441、化合物

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

1.90 g of methyl 3-benzoylacrylate was dissolved in 30 ml of diethyl ether, and 0.8 ml of thioacetic acid was added thereto. The mixture was stirred for 5 hours at room temperature. The reaction solution was washed, in turn, with water, a saturated aqueous solution of sodium hydrogencarbonate and water, and dried over magnesium sulfate. The diethyl ether was removed from the solution by evaporation, and the residue was purified by silica gel column chromatography using a mixture of hexane and diethyl ether as an eluent, and then recrystallized from the same mixture to give 2.42 g of methyl 2-acetylthio-3-benzoylpropionate.

後処理

  1. washThe reaction solution was washed, in turn, with water
  2. dry with materiala saturated aqueous solution of sodium hydrogencarbonate and water, and dried over magnesium sulfate
  3. customThe diethyl ether was removed from the solution by evaporation
  4. customthe residue was purified by silica gel column chromatography
  5. additiona mixture of hexane and diethyl ether as an eluent
  6. customrecrystallized from the same mixture

出典と根拠

ORDレコード
ord-08391010ad0b45479b52f0b2621adecc
出典データセット
uspto-grants-1986_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04594197

反応ノート

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