Ethylene Glycol → 1-Fluoro-3,7,11-trimethyldodeca-2,4,10-triene

HRID 918335ノート

反応式

HRID 918335 の反応式
Br[CH2:2][CH:3]=[C:4]([CH3:16])[CH:5]=[CH:6][CH2:7][CH:8]([CH3:15])[CH2:9][CH2:10][CH:11]=[C:12]([CH3:14])[CH3:13].C(O)CO.[F-:21].[K+]>CCOCC>[F:21][CH2:2][CH:3]=[C:4]([CH3:16])[CH:5]=[CH:6][CH2:7][CH:8]([CH3:15])[CH2:9][CH2:10][CH:11]=[C:12]([CH3:14])[CH3:13]

参加物

5

反応物 3

HCID 174Ethylene Glycol2 回HCID 522689Potassium FluorideHCID 54370561HCID 54370561、化合物

生成物 1

HCID 538734921-Fluoro-3,7,11-trimethyldodeca-2,4,10-triene

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

A mixture of 33 g. of 1-bromo-3,7,11-trimethyldodeca-2,4,10-triene and 100 ml. of dry ethylene glycol is slowly added with stirring, to a suspension of 11.5 g. of potassium fluoride in 30 ml. of dry ethylene glycol and heated to about 120°, under an inert atmosphere. When addition is completed, the reaction mixture is stirred for about an additional 16 hours while maintaining the temperature at 120°. Then the mixture is cooled and 200 ml. of ether added. The mixture is washed thoroughly with water and the ether phase dried over sodium sulfate and solvent evaporated under reduced pressure to yield 1-fluoro-3,7,11-trimethyldodeca-2,4,10-triene.

後処理

  1. additionA mixture of 33 g
  2. additionWhen addition
  3. stirringthe reaction mixture is stirred for about an additional 16 hours
  4. temperaturewhile maintaining the temperature at 120°
  5. temperatureThen the mixture is cooled
  6. washThe mixture is washed thoroughly with water
  7. dry with materialthe ether phase dried over sodium sulfate and solvent
  8. customevaporated under reduced pressure

出典と根拠

ORDレコード
ord-0c27b4a3e06e4a76b667563f1bd9c9ca
出典データセット
uspto-grants-1976_07
特許番号
US03970704

反応ノート

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