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

HRID 981268
ノート
印刷プレビュー

反応式

HRID 981268 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

11

反応物 5

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

生成物 1

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

試薬・触媒・溶媒 5

HCID 244Benzyl Alcohol溶媒HCID 962Water溶媒HCID 8471Triethylamine溶媒HCID 8857Ethyl Acetate溶媒HCID 312751,4-Dioxane溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-c9ed52d6321e430f91821751adce7c10
出典データセット
uspto-grants-1991_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04990508

反応ノート

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