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6-(But-3-en-1-yl)-3-ethoxycyclohex-2-en-1-one → 4-(But-3-en-1-yl)cyclohex-2-en-1-one

HRID 1758160
ノート
印刷プレビュー

反応式

HRID 1758160 の反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH2:7]([CH:11]1[C:16](=O)[CH:15]=[C:14]([O:18]CC)[CH2:13][CH2:12]1)[CH2:8][CH:9]=[CH2:10]>CCOCC>[CH2:7]([CH:11]1[CH2:16][CH2:15][C:14](=[O:18])[CH:13]=[CH:12]1)[CH2:8][CH:9]=[CH2:10]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 127883066-(But-3-en-1-yl)-3-ethoxycyclohex-2-en-1-oneHCID 21226445Aluminium lithium hydride

生成物 1

HCID 127883074-(But-3-en-1-yl)cyclohex-2-en-1-one収率 78%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

実験手順

To a 0° C. slurry of 1.06 g. (26 mmoles) of lithium aluminum hydride in 75 ml. of ether was added a solution of 10 g. (51 mmoles) of 6-(3-butenyl)-3-ethoxy-2cyclohexen-1-one in 25 ml. of ether. After stirring for one hour, the reaction was quenched by addition of 100 ml. of 2 N hydrochloric acid. The quenched mixture was stirred for 30 minutes and then extracted with 300 ml. of ether. The ether extract was washed with 250 ml. saturated sodium bicarbonate, dried over magnesium sulfate and evaporated on a rotovapor. Distillation of the crude oil gave 5.98 g. (78%) of the title product.

後処理

  1. customTo a 0° C.
  2. customthe reaction was quenched by addition of 100 ml
  3. stirringThe quenched mixture was stirred for 30 minutes
  4. extractionextracted with 300 ml
  5. extractionThe ether extract
  6. washwas washed with 250 ml
  7. dry with materialsaturated sodium bicarbonate, dried over magnesium sulfate
  8. customevaporated on a rotovapor
  9. distillationDistillation of the crude oil
  10. customgave 5.98 g

出典と根拠

ORDレコード
ord-41c79b40e25c42dcacf785cceb656e55
出典データセット
uspto-grants-1983_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04371720

反応ノート

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