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Hydrochloric Acid → Methyl 4-(1-benzyloxycarbonylaminocyclopropyl)-2,3,5,6-tetrafluorobenzoate

HRID 981268
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HRID 981268 반응식
C([C:4]1([C:7]2[C:16]([F:17])=[C:15]([F:18])[C:10]([C:11]([O:13][CH3:14])=[O:12])=[C:9]([F:19])[C:8]=2[F:20])[CH2:6][CH2:5]1)(O)=O.C(Cl)(=O)[O:22][CH2:23][CH3:24].[N-]=[N+]=[N-].[Na+].Cl.C[N:33](C)[CH:34]=[O:35]>O1CCOCC1.C(O)C1C=CC=CC=1.O.C(OCC)(=O)C.C(N(CC)CC)C>[CH2:23]([O:22][C:34]([NH:33][C:4]1([C:7]2[C:8]([F:20])=[C:9]([F:19])[C:10]([C:11]([O:13][CH3:14])=[O:12])=[C:15]([F:18])[C:16]=2[F:17])[CH2:5][CH2:6]1)=[O:35])[C:24]1[CH:8]=[CH:7][CH:4]=[CH:5][CH:6]=1
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참가 물질

11

반응물 5

HCID 313Hydrochloric AcidHCID 6228DimethylformamideHCID 10928Ethyl chloroformateHCID 33557Sodium AzideHCID 15136257Methyl 4-(1-carboxycyclopropyl)-2,3,5,6-tetrafluorobenzoate

생성물 1

HCID 15136259Methyl 4-(1-benzyloxycarbonylaminocyclopropyl)-2,3,5,6-tetrafluorobenzoate수율 86.9%

시약·촉매·용매 5

HCID 244Benzyl Alcohol용매HCID 962Water용매HCID 8471Triethylamine용매HCID 8857Ethyl Acetate용매HCID 312751,4-Dioxane용매

실험 절차

In 90 ml of N,N-dimethylformamide was dissolved 9.0 g of methyl 4-(1-carboxycyclopropyl)-2,3,5,6-tetrafluorobenzoate. To the resulting solution were added, with ice-cooling, 4.0 g of ethyl chlorocarbonate and 3.7 g of triethylamine in this order. The resulting mixture was stirred at the same temperature for 30 minutes. Then, 2.6 g of sodium azide was added thereto with ice-cooling. The resulting mixture was stirred at the same temperature for 1 hour. To the reaction mixture were added 150 ml of ethyl acetate and 300 ml of water in this order. The resulting mixture was adjusted to pH 1 with 2N hydrochloric acid. The organic layer was separated, washed with water and a saturated aqueous sodium chloride solution in this order, and dried over anhydrous magnesium sulfate. The solvent was removed by distillation under reduced pressure. The residue obtained was dissolved in a mixture of 90 ml of dioxane and 8.1 g of benzyl alcohol. The resulting solution was refluxed for 1 hour. The reaction mixture was concentrated under reduced pressure. The residue obtained was purified by a column chromatography (eluant: toluene) to obtain 10.6 g (yield: 86.9%) of methyl 4-(1-benzyloxycarbonylaminocyclopropyl)-2,3,5,6-tetrafluorobenzoate.

후처리

  1. additionTo the resulting solution were added, with ice-
  2. temperaturecooling
  3. temperaturewith ice-cooling
  4. stirringThe resulting mixture was stirred at the same temperature for 1 hour
  5. customThe organic layer was separated
  6. washwashed with water
  7. dry with materiala saturated aqueous sodium chloride solution in this order, and dried over anhydrous magnesium sulfate
  8. customThe solvent was removed by distillation under reduced pressure
  9. customThe residue obtained
  10. temperatureThe resulting solution was refluxed for 1 hour
  11. concentrationThe reaction mixture was concentrated under reduced pressure
  12. customThe residue obtained
  13. customwas purified by a column chromatography (eluant: toluene)

출처 및 근거

ORD 기록
ord-c9ed52d6321e430f91821751adce7c10
출처 데이터셋
uspto-grants-1991_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04990508

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