Hydrochloric Acid → HCID 23158218、化合物

HRID 601642ノート

反応式

HRID 601642 の反応式
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]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 63651,1-Dichloroethane3 回HCID 6882252-Bromo-3,5-dimethoxy-1-fluorobenzeneHCID 2757989Cyclohexylacetyl chloride

生成物 1

HCID 23158218HCID 23158218、化合物収率 22.2%

試薬・触媒・溶媒 1

HCID 3007855Zincchloride触媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-29dd371dbeab4b048706b212ca484592
出典データセット
uspto-grants-2011_03
特許番号
US07902369B2

反応ノート

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