Acetic Acid → 7-Isopropoxy-5-methyl-4-heptenal

HRID 1581081ノート

反応式

HRID 1581081 の反応式
[CH:1]([O:4][CH2:5][CH2:6][C:7]([CH3:11])(O)[CH:8]=[CH2:9])([CH3:3])[CH3:2].[C:12](O)(=[O:14])[CH3:13].C(=O)([O-])[O-].[K+].[K+]>C(OCC)=C>[CH:1]([O:4][CH2:5][CH2:6][C:7]([CH3:11])=[CH:8][CH2:9][CH2:13][CH:12]=[O:14])([CH3:3])[CH3:2]

参加物

5

反応物 3

HCID 176Acetic AcidHCID 11430Potassium CarbonateHCID 23263480HCID 23263480、化合物

生成物 1

HCID 540432947-Isopropoxy-5-methyl-4-heptenal

試薬・触媒・溶媒 1

HCID 8023Ethyl vinyl ether溶媒

実験手順

15.8 g (0.1 mol) of 5-isopropoxy-3-methyl-1-penten-3-ol and 20.0 g of mercuric acetate in 180 cc of ethyl vinyl ether are maintained at reflux temperature over the course of 4 days. 0.9 cc of glacial acetic acid is added at 20° to the turbid solution. After 3 hours 150 cc of 5 % potassium carbonate solution are added and the product is extracted with hexane. The hexane extract is dried with sodium sulphate and evaporated. The residue is heated to 165°-168° over the course of 11/2 hours without further purification and in an atomosphere of nitrogen; the residue is subsequently distilled at reduced pressure. The 7-isopropoxy-5-methyl-4-heptenal has a B.P. of 70°-73°/0.8 mm.

後処理

  1. temperatureat reflux temperature over the course of 4 days
  2. extractionthe product is extracted with hexane
  3. extractionThe hexane extract
  4. dry with materialis dried with sodium sulphate
  5. customevaporated
  6. temperatureThe residue is heated to 165°-168° over the course of 11/2 hours without further purification and in an atomosphere of nitrogen
  7. distillationthe residue is subsequently distilled at reduced pressure

出典と根拠

ORDレコード
ord-ba7da04080f44ff3a9bee06c93599057
出典データセット
uspto-grants-1976_01
特許番号
US03935271

反応ノート

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