Isodecanol → (2E)-2-Bromo-2-butenedioic acid

HRID 1638399ノート

反応式

HRID 1638399 の反応式
[Br:1][C:2]1[C:3]([O:5][C:6](=[O:8])[CH:7]=1)=[O:4].C([OH:19])CCCCCCC(C)C>C1(C)C=CC=CC=1>[Br:1]/[C:2](=[CH:7]/[C:6]([OH:5])=[O:8])/[C:3]([OH:19])=[O:4]

参加物

4

反応物 2

HCID 32898IsodecanolHCID 800273-Bromo-2,5-furandione

生成物 1

HCID 5358119(2E)-2-Bromo-2-butenedioic acid収率 260.6%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

Bromomaleic anhydride (19.5 g), isodecanol (69.5 g) p-toluene sulphonic acid (2 g) and toluene (70 ml) were stirred and boiled under reflux below a Dean-Stark trap of volume 15 ml for 2.5 hours. The solution was then cooled with petroleum ether and the petroleum ether solution was washed with water. The solvent and excess isodecanol were distilled under reduced pressure, finally at 100°/0.2 mm of mercury pressure, leaving the bis(isodecyl)ester of bromomaleic acid (56 g) as an oil with an estimated purity by gas chromatography of 96%.

後処理

  1. temperatureunder reflux below a Dean-Stark trap of volume 15 ml for 2.5 hours
  2. washthe petroleum ether solution was washed with water
  3. distillationThe solvent and excess isodecanol were distilled under reduced pressure, finally at 100°/0.2 mm of mercury pressure

出典と根拠

ORDレコード
ord-fc4d7f45591345f59d6dc424cf8adbb2
出典データセット
uspto-grants-1989_11
特許番号
US04879388

反応ノート

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