Hydrochloric Acid → HCID 11179971, 화합물

HRID 1822295노트

반응식

HRID 1822295 반응식
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]

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 57894208HCID 57894208, 화합물

생성물 1

HCID 11179971HCID 11179971, 화합물수율 109.9%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-4aff6617075a4222b3f84d4869dbf421
출처 데이터셋
uspto-grants-2009_10
특허 번호
US07608639B2

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