Hydrochloric Acid → HCID 23158218, 화합물

HRID 601642노트

반응식

HRID 601642 반응식
ClC(Cl)C.[Br:5][C:6]1[C:11]([O:12][CH3:13])=[CH:10][C:9]([O:14][CH3:15])=[CH:8][C:7]=1[F:16].[CH:17]1([CH2:23][C:24](Cl)=[O:25])[CH2:22][CH2:21][CH2:20][CH2:19][CH2:18]1.Cl>[Cl-].[Cl-].[Zn+2]>[Br:5][C:6]1[C:7]([F:16])=[C:8]([C:24](=[O:25])[CH2:23][CH:17]2[CH2:22][CH2:21][CH2:20][CH2:19][CH2:18]2)[C:9]([O:14][CH3:15])=[CH:10][C:11]=1[O:12][CH3:13]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 63651,1-Dichloroethane3회HCID 6882252-Bromo-3,5-dimethoxy-1-fluorobenzeneHCID 2757989Cyclohexylacetyl chloride

생성물 1

HCID 23158218HCID 23158218, 화합물수율 22.2%

시약·촉매·용매 1

HCID 3007855Zincchloride촉매

실험 절차

Under nitrogen atmosphere, 6 ml of dichloroethane solution with 2.3 g of 2-bromo-3,5-dimethoxy-1-fluorobenzene and 6 ml of dichloroethane solution with 2.3 g of cyclohexylacetylchloride were dropped sequentially to 15 ml of dichloroethane solution with 1.8 g of alminium trichloride, 180 mg of zinc dichloride at −10° C., and then the mixture was stirred at room temperature for 2 hours. 20% of hydrochloric acid solution was added to the reaction solution, extracted with chloroform. Chloroform layer was washed with saturated saline solution and then dried with anhydrous sodium sulfate. After distilling out the solvents under reduced pressure, residues were separated and purified with silicagel chromatography (hexane/ethyl acetate=5/1) to obtain 780 mg of the above compound as a white solid.

후처리

  1. extractionextracted with chloroform
  2. washChloroform layer was washed with saturated saline solution
  3. dry with materialdried with anhydrous sodium sulfate
  4. distillationAfter distilling out the solvents under reduced pressure, residues
  5. customwere separated
  6. custompurified with silicagel chromatography (hexane/ethyl acetate=5/1)

출처 및 근거

ORD 기록
ord-29dd371dbeab4b048706b212ca484592
출처 데이터셋
uspto-grants-2011_03
특허 번호
US07902369B2

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