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Citric Acid → (5-chloro-2-fluoro-4-((1,2-dimethyl-1H-3-indolylcarbonyl)amino)phenyl)acetic acid

HRID 1372716
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HRID 1372716 반응식
[CH3:1][N:2]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[C:4]([C:11]([OH:13])=O)=[C:3]1[CH3:14].C(Cl)(=O)C(Cl)=O.C(N(CC)CC)C.[NH2:28][C:29]1[CH:34]=[C:33]([F:35])[C:32]([CH2:36][C:37]([O:39]CC)=[O:38])=[CH:31][C:30]=1[Cl:42].C1C=CC2N(O)N=NC=2C=1.C(O)(=O)CC(CC(O)=O)(C(O)=O)O.[OH-].[Na+].Cl>C(Cl)Cl.C(Cl)(Cl)Cl>[Cl:42][C:30]1[C:29]([NH:28][C:11]([C:4]2[C:5]3[C:10](=[CH:9][CH:8]=[CH:7][CH:6]=3)[N:2]([CH3:1])[C:3]=2[CH3:14])=[O:13])=[CH:34][C:33]([F:35])=[C:32]([CH2:36][C:37]([OH:39])=[O:38])[CH:31]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

11

반응물 8

HCID 311Citric AcidHCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 14798Sodium HydroxideHCID 65578Oxalyl chlorideHCID 757711-HydroxybenzotriazoleHCID 27610321,2-Dimethylindole-3-carboxylic acid
HCID 17858807
Ethyl 4-amino-5-chloro-2-fluorophenylacetate

생성물 1

HCID 17859113(5-chloro-2-fluoro-4-((1,2-dimethyl-1H-3-indolylcarbonyl)amino)phenyl)acetic acid수율 50.3%

시약·촉매·용매 2

HCID 6212Chloroform용매HCID 6344Dichloromethane용매2회

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온도
0 °C

실험 절차

In methylene chloride (8 ml) was dissolved 1,2-dimethyl-1H-indole-3-carboxylic acid (270 mg, 1.43 mmol) was dissolved. Oxalyl chloride (0.19 ml, 2.1 mmol) was added to the solution under stirring at 0° C. The reaction mixture was stirred at room temperature for 1 hour and distilled under reduced pressure to remove the solvent. The residue was dissolved in methylene chloride (6 ml) and the resulting solution was added to a solution of triethylamine (0.56 ml, 4.3 mmol) and ethyl (4-amino-3-chloro-6-fluorophenyl)acetate (331 mg, 1.4 mmol) in methylene chloride (3 ml) under stirring at 0° C. The reaction mixture was heated at reflux for 18 hours. HOBt (catalytic amount) was added to the reaction mixture and the mixture was heated under reflux for 48 hours. After cooling, the reaction mixture was added with chloroform and a saturated aqueous solution of citric acid. The mixture was extracted with chloroform. The extract was washed with saturated brine, dried over anhydrous sodium sulfate and distilled under reduced pressure to remove the solvent. The residue was purified by silica gel column chromatography (middle pressure Yamazen, linear gradient of n-hexane/ethyl acetate form 9:1 to 7:3, 20 ml/min, φ 50 mm×150 mm, dry silica gel adsorption method). The purified product was dissolved in THF (15 ml) and to the resulting solution was added 0.25M NaOH (8.6 ml, 2.2 mmol). The mixture was stirred at room temperature for 18 hours. The reaction mixture was poured into 1M HCl to acidify therewith. The crystals thus precipitated were collected by filtration under reduced pressure, washed with water and dried under reduced pressure to give (5-chloro-2-fluoro-4-((1,2-dimethyl-1H-3-indolylcarbonyl)amino)phenyl)acetic acid (264 mg, 49%) as a colorless solid.

후처리

  1. dissolutionwas dissolved
  2. stirringThe reaction mixture was stirred at room temperature for 1 hour
  3. distillationdistilled under reduced pressure
  4. customto remove the solvent
  5. dissolutionThe residue was dissolved in methylene chloride (6 ml)
  6. stirringunder stirring at 0° C
  7. temperatureThe reaction mixture was heated
  8. temperatureat reflux for 18 hours
  9. temperaturethe mixture was heated
  10. temperatureunder reflux for 48 hours
  11. temperatureAfter cooling
  12. extractionThe mixture was extracted with chloroform
  13. washThe extract was washed with saturated brine
  14. dry with materialdried over anhydrous sodium sulfate
  15. distillationdistilled under reduced pressure
  16. customto remove the solvent
  17. customThe residue was purified by silica gel column chromatography (middle pressure Yamazen, linear gradient of n-hexane/ethyl acetate form 9:1 to 7:3, 20 ml/min, φ 50 mm×150 mm, dry silica gel adsorption method)
  18. dissolutionThe purified product was dissolved in THF (15 ml) and to the resulting solution
  19. stirringThe mixture was stirred at room temperature for 18 hours
  20. customThe crystals thus precipitated
  21. filtrationwere collected by filtration under reduced pressure
  22. washwashed with water
  23. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-56e6f87fe50343b1b852ddacde4779fb
출처 데이터셋
uspto-grants-2007_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07157487B2

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