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Sodium Hydroxide → 7-(4-Trifluoromethoxyphenyl)-2,3-dihydro-1-benzoxepine-4-carboxylic acid

HRID 1277186
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HRID 1277186 반응식
[F:1][C:2]([F:27])([F:26])[O:3][C:4]1[CH:9]=[CH:8][C:7]([C:10]2[CH:11]=[CH:12][C:13]3[O:19][CH2:18][CH2:17][C:16]([C:20]([O:22]CC)=[O:21])=[CH:15][C:14]=3[CH:25]=2)=[CH:6][CH:5]=1.[OH-].[Na+]>O1CCCC1CCO>[F:27][C:2]([F:1])([F:26])[O:3][C:4]1[CH:9]=[CH:8][C:7]([C:10]2[CH:11]=[CH:12][C:13]3[O:19][CH2:18][CH2:17][C:16]([C:20]([OH:22])=[O:21])=[CH:15][C:14]=3[CH:25]=2)=[CH:6][CH:5]=1
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참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 18472320Ethyl 7-(4-trifluoromethoxyphenyl)-2,3-dihydro-1-benzoxepine-4-carboxylate

생성물 1

HCID 184724787-(4-Trifluoromethoxyphenyl)-2,3-dihydro-1-benzoxepine-4-carboxylic acid수율 94%

시약·촉매·용매 1

HCID 119895722-(Oxolan-2-yl)ethan-1-ol용매

실험 절차

To a solution of ethyl 7-(4-trifluoromethoxyphenyl)-2,3-dihydro-1-benzoxepine-4-carboxylate (323.9 mg) in tetrahydrofuran-ethanol (5-5 ml) was added 1N sodium hydroxide (2.0 ml) at room temperature, and the mixture was stirred for 5 days and concentrated under reduced pressure. To the residue 1N hydrochloric acid (5 ml) was added, and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated sodium chloride solution, dried with magnesium sulfate and concentrated. The resulting crystal was collected by filtration to give 7-(4-trifluoromethoxyphenyl)-2,3-dihydro-1-benzoxepine-4-carboxylic acid (282 mg) as colorless crystals.

후처리

  1. concentrationconcentrated under reduced pressure
  2. additionTo the residue 1N hydrochloric acid (5 ml) was added
  3. extractionthe mixture was extracted with ethyl acetate
  4. washThe organic layer was washed with saturated sodium chloride solution
  5. dry with materialdried with magnesium sulfate
  6. concentrationconcentrated
  7. filtrationThe resulting crystal was collected by filtration

출처 및 근거

ORD 기록
ord-b0f8f191ff7a489182d07337cf47048e
출처 데이터셋
uspto-grants-2000_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06166006

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