Hydrochloric Acid → HCID 178496930, 화합물

HRID 1248359노트

반응식

HRID 1248359 반응식
[CH3:1][O:2][C:3]([C:5]1[C:8]2[CH:9]=[C:10]([O:22]C)[C:11]([C:13](=[O:21])[C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][C:15]=3[F:20])=[CH:12][C:7]=2[CH:6]=1)=[O:4].[Cl-].[Cl-].[Cl-].[Al+3].Cl>ClCCl>[CH3:1][O:2][C:3]([C:5]1[C:8]2[CH:9]=[C:10]([OH:22])[C:11]([C:13](=[O:21])[C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][C:15]=3[F:20])=[CH:12][C:7]=2[CH:6]=1)=[O:4]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 6451240Aluminum(III) ChlorideHCID 1784969314-(o-Fluorobenzoyl)-5-methoxybenzocyclobutene-1-carboxylic acid methyl ester

생성물 1

HCID 178496930HCID 178496930, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

5.0 g of 4-(o-fluorobenzoyl)-5-methoxybenzocyclobutene-1-carboxylic acid methyl ester are dissolved in 100 ml of dichloromethane; 6.4 g of aluminium trichloride are added and the whole is heated at boiling for 4 hours while stirring. The mixture is poured onto ice; 20 ml of concentrated hydrochloric acid are added and the whole is extracted by shaking twice with 100 ml of dichloromethane each time. The organic phases are combined, washed with water, dried over magnesium sulphate and concentrated to dryness by evaporation. The residue is chromatographed over silica gel and recrystallised from ether/hexane. 4-(o-fluorobenzoyl)-5-hydroxybenzocyclobutene-1-carboxylic acid methyl ester is obtained having a melting point of 72°-73°.

후처리

  1. temperaturethe whole is heated
  2. additionThe mixture is poured onto ice
  3. extractionthe whole is extracted
  4. stirringby shaking twice with 100 ml of dichloromethane each time
  5. washwashed with water
  6. dry with materialdried over magnesium sulphate
  7. concentrationconcentrated to dryness by evaporation
  8. customThe residue is chromatographed over silica gel
  9. customrecrystallised from ether/hexane

출처 및 근거

ORD 기록
ord-bdba3c636a094c28a38b372590845602
출처 데이터셋
uspto-grants-1985_06
특허 번호
US04523030

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