Methanol → Cyclohexylfulvene

HRID 1251529노트

반응식

HRID 1251529 반응식
[CH:1]1[CH2:5][CH:4]=[CH:3][CH:2]=1.[C:6]1(=O)[CH2:11][CH2:10][CH2:9][CH2:8][CH2:7]1.CO.N1CCC[CH2:16]1>O.C(O)(=O)C>[CH:6]1([C:2]2[C:1](=[CH2:16])[CH:5]=[CH:4][CH:3]=2)[CH2:11][CH2:10][CH2:9][CH2:8][CH2:7]1

참가 물질

7

반응물 4

HCID 887MethanolHCID 7612CyclopentadieneHCID 7967CyclohexanoneHCID 31268Pyrrolidine

생성물 1

HCID 22327799Cyclohexylfulvene수율 92.8%

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 962Water용매

실험 절차

8.2 ml (100 mmol) of cyclopentadiene and 4.2 ml (40 mmol) of cyclohexanone were added to 40 ml of dehydrated methanol, and 5.0 ml (60 mmol) of pyrrolidine were then added dropwise at 0° C. Then, reaction was carried out at room temperature for 3 hours. Next, 3.8 ml of acetic acid were slowly added at 0° C., and 20 ml of water were further added, followed by extraction with diethyl ether. The resultant organic phase, after washed with water, was dried over magnesium sulfate, and the used solvent was then distilled off to obtain 5.95 g of a yellow liquid.

후처리

  1. additionwere then added dropwise at 0° C
  2. customThen, reaction
  3. extractionfollowed by extraction with diethyl ether
  4. washThe resultant organic phase, after washed with water
  5. dry with materialwas dried over magnesium sulfate
  6. distillationthe used solvent was then distilled off

출처 및 근거

ORD 기록
ord-ac64bae7b4274fdc8052ee9019980cbe
출처 데이터셋
uspto-grants-2002_01
특허 번호
US06342568B1

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