Hydrochloric Acid → HCID 11555148、化合物

HRID 2076591ノート

反応式

HRID 2076591 の反応式
[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]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 67119193HCID 67119193、化合物

生成物 1

HCID 11555148HCID 11555148、化合物収率 82.3%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-5a7d364018bf4f6fa5a86168b9bb93ae
出典データセット
uspto-grants-2011_04
特許番号
US07923573B2

反応ノート

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