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

HRID 1387935
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반응식

HRID 1387935 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:9]=[CH:10][C:11]3[O:17][CH2:16][CH2:15][C:14]([C:18]([O:20]CC)=[O:19])=[CH:13][C:12]=3[CH:23]=2)=[CH:4][CH:3]=1.[OH-].[Na+]>O1CCCC1CCO>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[CH:9]=[CH:10][C:11]3[O:17][CH2:16][CH2:15][C:14]([C:18]([OH:20])=[O:19])=[CH:13][C:12]=3[CH:23]=2)=[CH:6][CH:7]=1
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참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 18472211Ethyl 7-(4-chlorophenyl)-2,3-dihydro-1-benzoxepine-4-carboxylate

생성물 1

HCID 184723867-(4-Chlorophenyl)-2,3-dihydro-1-benzoxepine-4-carboxylic acid수율 93.5%

시약·촉매·용매 1

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

실험 절차

To a solution of ethyl 7-(4-chlorophenyl)-2,3-dihydro-1-benzoxepine-4-carboxylate (400 mg) in tetrahydrofuran-ethanol (10-10 ml) was added 1N sodium hydroxide (2.0 ml) at room temperature, and the mixture was stirred for 42 hours and concentrated under reduced pressure. To the residue was added 1N hydrochloric acid (15 ml), 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-chlorophenyl)-2,3-dihydro-1-benzoxepine-4-carboxylic acid (342 mg) as colorless crystals.

후처리

  1. concentrationconcentrated under reduced pressure
  2. additionTo the residue was added 1N hydrochloric acid (15 ml)
  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-c6fbeb36b58c4c56b35f28676ebfb0a4
출처 데이터셋
uspto-grants-2001_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06268354B1

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