Hydrochloric Acid → 1-(2,5-Dimethoxy-4-chlorophenyl)-4-cyclohexyl-1-butanone

HRID 844420노트

반응식

HRID 844420 반응식
[CH2:1]1[CH2:6][CH2:5][CH:4]([CH2:7][CH2:8][CH2:9][C:10](Cl)=[O:11])[CH2:3][CH2:2]1.[Al+3].[Cl-].[Cl-].[Cl-].[CH3:17][O:18][C:19]1[CH:24]=[CH:23][C:22]([O:25][CH3:26])=[CH:21][C:20]=1[Cl:27].Cl>C(Cl)(Cl)(Cl)Cl>[CH:4]1([CH2:7][CH2:8][CH2:9][C:10]([C:23]2[CH:24]=[C:19]([O:18][CH3:17])[C:20]([Cl:27])=[CH:21][C:22]=2[O:25][CH3:26])=[O:11])[CH2:5][CH2:6][CH2:1][CH2:2][CH2:3]1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 2467242-Chloro-1,4-dimethoxybenzeneHCID 6451240Aluminum(III) ChlorideHCID 133156254-Cyclohexylbutanoyl chloride

생성물 1

HCID 226126531-(2,5-Dimethoxy-4-chlorophenyl)-4-cyclohexyl-1-butanone수율 51.9%

시약·촉매·용매 1

HCID 5943Carbon Tetrachloride용매3회

실험 절차

3.77 g of 4-cyclohexanebutyryl chloride dissolved in 10 ml of CCl4 are added to a suspension of 2.8 g of AlCl3 in 20 ml of CCl4 at +4° C. under nitrogen. 5.2 g of 2,5-dimethoxychlorobenzene in 10 ml of CCl4 are added dropwise and the mixture is then left stirring for 3 hours at RT. The reaction medium is hydrolysed with dilute HCl solution, the phases are then separated by settling and the organic phase is extracted with DCM. After drying over MgSO4, the solution is evaporated and the residue is then purified by chromatography on silica, eluting with a heptane/DCM mixture (60/40; v/v) and then with pure DCM. 3.37 g of the expected compound are obtained: m.p.=80-81° C.

후처리

  1. waitthe mixture is then left
  2. customthe phases are then separated
  3. extractionthe organic phase is extracted with DCM
  4. dry with materialAfter drying over MgSO4
  5. customthe solution is evaporated
  6. customthe residue is then purified by chromatography on silica
  7. washeluting with a heptane/DCM mixture (60/40; v/v)

출처 및 근거

ORD 기록
ord-ac165cf32ebe4d8f9d24d72089e56efb
출처 데이터셋
uspto-grants-2002_04
특허 번호
US06380230B1

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