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

HRID 1638399노트

반응식

HRID 1638399 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

HCID 5358119(2E)-2-Bromo-2-butenedioic acid수율 260.6%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

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%.

후처리

  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

출처 및 근거

ORD 기록
ord-fc4d7f45591345f59d6dc424cf8adbb2
출처 데이터셋
uspto-grants-1989_11
특허 번호
US04879388

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