2-Methyl-2-(pent-4-yn-1-yl)propanedioicacid → 2-Methylhept-6-ynoic acid

HRID 1197364

반응식

HRID 1197364 반응식
[CH3:1][C:2]([CH2:9][CH2:10][CH2:11][C:12]#[CH:13])(C(O)=O)[C:3]([OH:5])=[O:4]>C(#N)C>[CH3:1][CH:2]([CH2:9][CH2:10][CH2:11][C:12]#[CH:13])[C:3]([OH:5])=[O:4]

참가 물질

3

반응물 1

HCID 193733782-Methyl-2-(pent-4-yn-1-yl)propanedioicacid

생성물 1

HCID 193732982-Methylhept-6-ynoic acid수율 83%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

A mixture of 2-methyl-2-(pent-4-ynyl)malonic acid (5.7 g) and cuprous oxide (0.22 g) in acetonitrile (150 ml) was heated to reflux, under a nitrogen atmosphere, for 4.25 hours. The solvent was removed under reduced pressure and water (50 ml) was added to the residue followed by sufficient concentrated hydrochloric acid to hydrolyse the copper salts. The resulting aqueous phase was extracted with diethyl ether and the organic extracts were washed with water and brine before drying over anhydrous magnesium sulphate and evaporation in vacuo. 2-Methylhept-6-ynoic acid (3.6 g) was obtained as a colourless oil after distillation (b.p. 150°-165°, 0.5 mm Hg).

후처리

  1. temperaturewas heated
  2. temperatureto reflux, under a nitrogen atmosphere, for 4.25 hours
  3. customThe solvent was removed under reduced pressure and water (50 ml)
  4. additionwas added to the residue
  5. extractionThe resulting aqueous phase was extracted with diethyl ether
  6. washthe organic extracts were washed with water and brine
  7. dry with materialbefore drying over anhydrous magnesium sulphate and evaporation in vacuo

출처 및 근거

ORD 기록
ord-3e727cac35f640b383df5c84692b4630
출처 데이터셋
uspto-grants-1992_05
특허 번호
US05116862

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