Hydrochloric Acid → HCID 178444483, 화합물

HRID 2309301

반응식

HRID 2309301 반응식
[CH2:1]([C:3]1[CH:8]=[CH:7][C:6]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)=[C:5]([F:15])[CH:4]=1)[CH3:2].[Cl-].[Cl-].[Cl-].[Al+3].[CH2:20]([C@H:25]1[CH2:30][CH2:29][C@H:28]([CH2:31][C:32](Cl)=[O:33])[CH2:27][CH2:26]1)[CH2:21][CH2:22][CH2:23][CH3:24].Cl>ClCCl>[CH2:20]([C@H:25]1[CH2:26][CH2:27][C@H:28]([CH2:31][C:32]([C:12]2[CH:11]=[CH:10][C:9]([C:6]3[CH:7]=[CH:8][C:3]([CH2:1][CH3:2])=[CH:4][C:5]=3[F:15])=[CH:14][CH:13]=2)=[O:33])[CH2:29][CH2:30]1)[CH2:21][CH2:22][CH2:23][CH3:24]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 14903264-Ethyl-2-fluoro-1,1'-biphenylHCID 6451240Aluminum(III) ChlorideHCID 178444488HCID 178444488, 화합물

생성물 1

HCID 178444483HCID 178444483, 화합물수율 51.5%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

4-Ethyl-2-fluorobiphenyl (13.0 gram) was added in one portion to a stirred suspension of aluminium trichloride (9.54 gram) in dichloromethane (30 ml), followed by a solution of trans-4-n-pentylcyclohexyl acetyl chloride (15 gram) in dichloromethane (30 ml), added dropwise over 30 minutes. After stirring at room temperature for 31/2 hours, the reaction mixture was poured onto ice (250 gram) and hydrochloric acid (25 ml) and the product was extracted with 350 ml and 250 ml portions of petroleum ether (boiling point 60°-80° C.). The combined extracts were washed with water (150 ml), dried over anhydrous sodium sulphate and evaporated to dryness. The residue (26.8 gram) was crystallised from industrial methylated spirits at 0° C. to give 13.2 gram (51.5% yield) 4-(trans-4-n-pentylcyclohexylacetyl)-2'-fluoro-4'-ethylbiphenyl, melting point 72°-73° C.

후처리

  1. additionadded dropwise over 30 minutes
  2. extractionthe product was extracted with 350 ml and 250 ml portions of petroleum ether (boiling point 60°-80° C.)
  3. washThe combined extracts were washed with water (150 ml)
  4. dry with materialdried over anhydrous sodium sulphate
  5. customevaporated to dryness
  6. customThe residue (26.8 gram) was crystallised from industrial methylated spirits at 0° C.

출처 및 근거

ORD 기록
ord-a48c5a2205d64bc589a453973ad18110
출처 데이터셋
uspto-grants-1987_09
특허 번호
US04695131

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