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Hydrochloric Acid → 4-(1-Benzyloxycarbonylaminocyclopropyl)-2,3,5,6tetrafluorobenzoic acid

HRID 981274
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인쇄 미리보기

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HRID 981274 반응식
[CH2:1]([O:8][C:9]([NH:11][C:12]1([C:15]2[C:24]([F:25])=[C:23]([F:26])[C:18]([C:19]([O:21]C)=[O:20])=[C:17]([F:27])[C:16]=2[F:28])[CH2:14][CH2:13]1)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[OH-].[Na+].O.Cl>CO.O1CCOCC1.C(OCC)(=O)C>[CH2:1]([O:8][C:9]([NH:11][C:12]1([C:15]2[C:16]([F:28])=[C:17]([F:27])[C:18]([C:19]([OH:21])=[O:20])=[C:23]([F:26])[C:24]=2[F:25])[CH2:13][CH2:14]1)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 14798Sodium HydroxideHCID 15136259Methyl 4-(1-benzyloxycarbonylaminocyclopropyl)-2,3,5,6-tetrafluorobenzoate

생성물 1

HCID 100454814-(1-Benzyloxycarbonylaminocyclopropyl)-2,3,5,6tetrafluorobenzoic acid수율 97.9%

시약·촉매·용매 3

HCID 887
Methanol
용매
HCID 8857Ethyl Acetate용매
HCID 312751,4-Dioxane용매

실험 절차

In a mixture of 14 ml of methanol and 14 ml of dioxane was dissolved 1.8 g of methyl 4-(1-benzyloxycarbonylaminocyclopropyl)-2,3,5,6-tetrafluorobenzoate. To the resulting solution was added 14 ml of a 1N aqueous sodium hydroxide solution. The resulting mixture was stirred at room temperature for 1 hour. To the reaction mixture was added 50 ml of water. The resulting mixture was adjusted to pH 1 with 2N hydrochloric acid, and 50 ml of ethyl acetate was added thereto. 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, and n-hexane was added to the residue obtained. The resulting crystals were collected by filtration to obtain 1.7 g (yield: 97.7%) of 4-(1-benzyloxycarbonylaminocyclopropyl)-2,3,5,6tetrafluorobenzoic acid.

후처리

  1. additionwas added
  2. customThe organic layer was separated
  3. washwashed with water
  4. dry with materiala saturated aqueous sodium chloride solution in this order, and dried over anhydrous magnesium sulfate
  5. customThe solvent was removed by distillation under reduced pressure, and n-hexane
  6. additionwas added to the residue
  7. customobtained
  8. filtrationThe resulting crystals were collected by filtration

출처 및 근거

ORD 기록
ord-8742601296844af4835a876469d549af
출처 데이터셋
uspto-grants-1991_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04990508

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