Ethyl Acetate → 1-Benzyl-3-[4-(4-ethoxyphenyl)-4-methylpent-1-en-1-yl]benzene

HRID 1194411노트

반응식

HRID 1194411 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].[Cl-].[Al+3].[Cl-].[Cl-].[C:11]([C:19]1[CH:20]=[C:21]([CH:25]=[CH:26][CH2:27][C:28]([C:31]2[CH:36]=[CH:35][C:34]([O:37][CH2:38][CH3:39])=[CH:33][CH:32]=2)([CH3:30])[CH3:29])[CH:22]=[CH:23][CH:24]=1)(=O)[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1.C(OCC)(=O)C>CCOCC>[CH2:11]([C:19]1[CH:20]=[C:21]([CH:25]=[CH:26][CH2:27][C:28]([C:31]2[CH:36]=[CH:35][C:34]([O:37][CH2:38][CH3:39])=[CH:33][CH:32]=2)([CH3:30])[CH3:29])[CH:22]=[CH:23][CH:24]=1)[C:12]1[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=1

참가 물질

6

반응물 4

HCID 8857Ethyl AcetateHCID 6451240Aluminum(III) ChlorideHCID 21226445Aluminium lithium hydrideHCID 53914085{3-[4-(4-Ethoxyphenyl)-4-methylpent-1-en-1-yl]phenyl}(phenyl)methanone

생성물 1

HCID 544511461-Benzyl-3-[4-(4-ethoxyphenyl)-4-methylpent-1-en-1-yl]benzene수율 86.5%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매3회

실험 절차

To 5 ml of dry ether was added 0.1 g of lithium aluminum hydride, and thereinto was added a solution of 0.7 g of aluminum chloride in 10 ml of dry ether. A solution of 0.54 g of 1-(3-benzoylphenyl)-4-(4-ethoxyphenyl)-4-methyl-1-pentene (prepared according to (1) of Synthesis Example 12) in 2 ml of dry ether was added dropwise into the mixture, and refluxed for 30 minutes. After cooling to room temperature, ethyl acetate was added dropwise into the mixture. And the mixture was poured into ice water, and extracted with benzene. The benzene extract was washed with water and dried, and evaporated under reduced pressure, and purified by column chromatography on silica gel (1:2 mixed solvent of benzene and hexane) to give 0.45 g of the desired product.

후처리

  1. temperaturerefluxed for 30 minutes
  2. extractionextracted with benzene
  3. extractionThe benzene extract
  4. washwas washed with water
  5. customdried
  6. customevaporated under reduced pressure
  7. custompurified by column chromatography on silica gel (1:2 mixed solvent of benzene and hexane)

출처 및 근거

ORD 기록
ord-171f77f10e3543f197ecb80481b96349
출처 데이터셋
uspto-grants-1989_03
특허 번호
US04814340

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