Dichloromethane → 4-Cyclohexyl-1-(2,5-diethoxy-4-methylphenyl)butan-1-one

HRID 844421노트

반응식

HRID 844421 반응식
[CH:1]1([CH2:7][CH2:8][CH2:9][C:10](Cl)=[O:11])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[Al+3].[Cl-].[Cl-].[Cl-].[CH2:17]([O:19][C:20]1[CH:25]=[CH:24][C:23]([O:26][CH2:27][CH3:28])=[CH:22][C:21]=1[CH3:29])[CH3:18].C(Cl)Cl>C(Cl)(Cl)(Cl)Cl>[CH:1]1([CH2:7][CH2:8][CH2:9][C:10]([C:24]2[CH:25]=[C:20]([O:19][CH2:17][CH3:18])[C:21]([CH3:29])=[CH:22][C:23]=2[O:26][CH2:27][CH3:28])=[O:11])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1

참가 물질

6

반응물 4

HCID 6344DichloromethaneHCID 6451240Aluminum(III) ChlorideHCID 123535631,4-Diethoxy-2-methylbenzeneHCID 133156254-Cyclohexylbutanoyl chloride

생성물 1

HCID 226125564-Cyclohexyl-1-(2,5-diethoxy-4-methylphenyl)butan-1-one수율 75.6%

시약·촉매·용매 1

HCID 5943Carbon Tetrachloride용매3회

실험 절차

4 g of 4-cyclohexylbutyryl chloride dissolved in 10 ml of CCl4 are added to a suspension of 2.9 g of AlCl3 in 40 ml of CCl4 at +4° C. 4.2 g of 2,5-diethoxytoluene in 20 ml of CCl4 are added dropwise. After 4 hours at +4° C., the reaction medium is poured into dilute ice-cold HCl solution. DCM is added, the phases are separated out by settling and the organic phase is then dried over MgSO4. After evaporation of the solvent, the product is purified by chromatography on silica H, eluting with toluene. 5.33 g of the expected compound are obtained: m.p.=49-50° C.

후처리

  1. additionthe reaction medium is poured into dilute ice-cold HCl solution
  2. customthe phases are separated out
  3. dry with materialthe organic phase is then dried over MgSO4
  4. customAfter evaporation of the solvent
  5. customthe product is purified by chromatography on silica H
  6. washeluting with toluene

출처 및 근거

ORD 기록
ord-c1c8274ccb214c52ac9c0e02c689be9e
출처 데이터셋
uspto-grants-2002_04
특허 번호
US06380230B1

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