Hydrochloric Acid → HCID 11555148, 화합물

HRID 2076591노트

반응식

HRID 2076591 반응식
[OH-].[Na+].[OH:3][C:4]1[C:16]([C:17]([F:20])([F:19])[F:18])=[CH:15][CH:14]=[C:13]([CH2:21][O:22][C:23]2[CH:28]=[CH:27][C:26]([C:29]3[CH:34]=[CH:33][C:32]([CH2:35][C:36]([O:38]C)=[O:37])=[CH:31][CH:30]=3)=[CH:25][CH:24]=2)[C:5]=1[C:6]([O:8][C:9]([CH3:12])([CH3:11])[CH3:10])=[O:7].Cl>O1CCCC1>[C:9]([O:8][C:6]([C:5]1[C:4]([OH:3])=[C:16]([C:17]([F:18])([F:19])[F:20])[CH:15]=[CH:14][C:13]=1[CH2:21][O:22][C:23]1[CH:24]=[CH:25][C:26]([C:29]2[CH:34]=[CH:33][C:32]([CH2:35][C:36]([OH:38])=[O:37])=[CH:31][CH:30]=2)=[CH:27][CH:28]=1)=[O:7])([CH3:12])([CH3:10])[CH3:11]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 67119193HCID 67119193, 화합물

생성물 1

HCID 11555148HCID 11555148, 화합물수율 82.3%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A 3N aqueous sodium hydroxide solution (0.33 ml, 0.33 mmol) was added to a solution of tert-butyl 2-hydroxy-6-[({4′-[(methoxycarbonyl)methyl]-1,1′-biphenyl-4-yl}oxy)methyl]-3-(trifluoromethyl)benzoate (467 mg, 0.90 mmol) obtained in Example (6-9) in tetrahydrofuran (8 ml), and the mixture was stirred at room temperature for 10 hours. After the reaction mixture was poured into 1N hydrochloric acid and the mixture was extracted with ethyl acetate (three times), the organic layer was successively washed with water and a saturated aqueous NaCl solution and dried with anhydrous sodium sulfate. The solid obtained by removing the solvent under reduced pressure was reprecipitated using n-hexane-ethyl acetate to give the title compound as a white powder (372 mg, yield: 82%).

후처리

  1. extractionthe mixture was extracted with ethyl acetate (three times)
  2. washthe organic layer was successively washed with water
  3. dry with materiala saturated aqueous NaCl solution and dried with anhydrous sodium sulfate
  4. customThe solid obtained
  5. customby removing the solvent under reduced pressure
  6. customwas reprecipitated

출처 및 근거

ORD 기록
ord-5a7d364018bf4f6fa5a86168b9bb93ae
출처 데이터셋
uspto-grants-2011_04
특허 번호
US07923573B2

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