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Hydrochloric Acid → HCID 15670192, 화합물

HRID 248682
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HRID 248682 반응식
[Na+].C([S:5][CH2:6][CH:7]([CH2:20][C:21]1[CH:26]=[CH:25][C:24]([F:27])=[CH:23][CH:22]=1)[C:8]([NH:10][C:11]1[CH:12]=[C:13]([CH:17]=[CH:18][CH:19]=1)[C:14]([O-:16])=[O:15])=[O:9])(=O)C.[OH-].[Na+].Cl>O>[SH:5][CH2:6][CH:7]([CH2:20][C:21]1[CH:22]=[CH:23][C:24]([F:27])=[CH:25][CH:26]=1)[C:8]([NH:10][C:11]1[CH:12]=[C:13]([CH:17]=[CH:18][CH:19]=1)[C:14]([OH:16])=[O:15])=[O:9]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 23701009HCID 23701009, 화합물

생성물 1

HCID 15670192HCID 15670192, 화합물수율 59.6%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

3-[[2-Acetylthiomethyl-3-(4-fluorophenyl)-propionyl]amino]benzoic acid sodium salt (compound of Example 40) (1.2 g) is dissolved in water (20 ml), and the mixture is adjusted to pH 12.0 with 10% aqueous sodium hydroxide solution under nitrogen. After reacting at room temperature for one hour, the reaction mixture is adjusted to pH 2.5 with 10% hydrochloric acid. The mixture is extracted with ethyl acetate (50 ml). The extract is washed with water and ethyl acetate is distilled off. The residue is purified by a medium pressure column chromatography with CHP-20P (eluant, water-dioxane). The fractions containing the desired compound are collected and lyophilized to give the title compound (0.6 g).

후처리

  1. extractionThe mixture is extracted with ethyl acetate (50 ml)
  2. washThe extract is washed with water and ethyl acetate
  3. distillationis distilled off
  4. customThe residue is purified by a medium pressure column chromatography with CHP-20P (eluant, water-dioxane)
  5. additionThe fractions containing the desired compound
  6. customare collected

출처 및 근거

ORD 기록
ord-f90927cb7ff0490ba326d2b268d4d0ed
출처 데이터셋
uspto-grants-1993_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05210266

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