Potassium Hydroxide → [5-(3-Methylbutoxy)-2-propylphenylthio] fumaric acid

HRID 1606106ノート

反応式

HRID 1606106 の反応式
[CH3:1][CH:2]([CH3:16])[CH2:3][CH2:4][O:5][C:6]1[CH:7]=[CH:8][C:9]([CH2:13][CH2:14][CH3:15])=[C:10]([SH:12])[CH:11]=1.[OH-].[K+].[K+].[C:20]([C:25]([O-:27])=[O:26])#[C:21][C:22]([OH:24])=[O:23]>O>[CH3:1][CH:2]([CH3:16])[CH2:3][CH2:4][O:5][C:6]1[CH:7]=[CH:8][C:9]([CH2:13][CH2:14][CH3:15])=[C:10]([S:12]/[C:21](=[CH:20]\[C:25]([OH:27])=[O:26])/[C:22]([OH:24])=[O:23])[CH:11]=1

参加物

5

反応物 3

HCID 14797Potassium HydroxideHCID 215459855-(3-Methylbutoxy)-2-propylthiophenolHCID 236779642-Butynedioic acid, monopotassium salt

生成物 1

HCID 86733255[5-(3-Methylbutoxy)-2-propylphenylthio] fumaric acid

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A solution of 95.7 parts of 5-(3-methylbutoxy)-2-propylthiophenol, 54 parts of potassium hydroxide and 73 parts of acetylene dicarboxylic acid mono potassium salt in 350 parts of water was refluxed for 40 minutes and cooled. The mixture was filtered through Whatman 54 filter paper to remove an oil residue and the filtrate was acidified to pH 1 with concentrated hydrochloric acid. The resulting yellow precipitate was collected, washed with water and dried in vacuo to give 67.8 parts of the desired product as a yellow powder, mp 121° - 129°C Crystallization from 15% ethanol-water afforded pure [5-(3-methylbutoxy)-2-propylphenylthio] fumaric acid, m.p. 131° - 133°C.

後処理

  1. temperaturecooled
  2. filtrationThe mixture was filtered through Whatman 54
  3. filtrationfilter paper
  4. customto remove an oil residue
  5. customThe resulting yellow precipitate was collected
  6. washwashed with water
  7. customdried in vacuo
  8. customto give
  9. custom67.8 parts of the desired product as a yellow powder, mp 121° - 129°C Crystallization from 15% ethanol-water afforded pure [5-(3-methylbutoxy)-2-propylphenylthio] fumaric acid, m.p. 131° - 133°C.

出典と根拠

ORDレコード
ord-ee2496d876034faaab063a1b7e507f35
出典データセット
uspto-grants-1976_04
特許番号
US03952013

反応ノート

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