Hydrochloric Acid → HCID 11179971、化合物

HRID 1822295ノート

反応式

HRID 1822295 の反応式
C([O:3][C:4](=[O:40])[CH2:5][CH2:6][C:7]1[CH:12]=[CH:11][C:10]([O:13][C:14]2[CH:19]=[C:18]([O:20][C:21]3[CH:26]=[CH:25][C:24]([C:27]([F:30])([F:29])[F:28])=[CH:23][C:22]=3[O:31][C:32]3[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=3)[CH:17]=[C:16]([CH3:38])[CH:15]=2)=[CH:9][C:8]=1[CH3:39])C.[OH-].[Na+].Cl>C(O)C.O>[CH3:39][C:8]1[CH:9]=[C:10]([O:13][C:14]2[CH:19]=[C:18]([O:20][C:21]3[CH:26]=[CH:25][C:24]([C:27]([F:30])([F:29])[F:28])=[CH:23][C:22]=3[O:31][C:32]3[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=3)[CH:17]=[C:16]([CH3:38])[CH:15]=2)[CH:11]=[CH:12][C:7]=1[CH2:6][CH2:5][C:4]([OH:40])=[O:3]

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 57894208HCID 57894208、化合物

生成物 1

HCID 11179971HCID 11179971、化合物収率 109.9%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

A solution of 3-{2-methyl-4-[3-methyl-5-(2-phenoxy-4-trifluoromethyl-phenoxy)-phenoxy]-phenyl}-propionic acid ethyl ester (0.137, 0.249 mmol) in ethanol (8 mL) is treated with 5 N NaOH (2 mL) and heated to reflux until saponification is completed. The mixture is cooled, and the solvent is removed in vacuo to afford a residue that is acidified with 1 N HCl. The mixture is diluted with water and extracted with ethyl acetate. The organic layer is dried (Na2SO4), and the solvent is removed in vacuo to afford 0.143 g (100%) of the title compound. 1H NMR (400 MHz, CDCl3); HRMS (ES+) m/z exact mass calculated for C30H25O5F3 523.1732, found 523.1721.

後処理

  1. temperatureheated
  2. temperatureto reflux until saponification
  3. temperatureThe mixture is cooled
  4. customthe solvent is removed in vacuo
  5. customto afford a residue that
  6. extractionextracted with ethyl acetate
  7. dry with materialThe organic layer is dried (Na2SO4)
  8. customthe solvent is removed in vacuo

出典と根拠

ORDレコード
ord-4aff6617075a4222b3f84d4869dbf421
出典データセット
uspto-grants-2009_10
特許番号
US07608639B2

反応ノート

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