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Oxalyl chloride → 3-(3-Fluorophenyl)-N-(3-hydroxy-2,6-dimethyl-phenyl)-5-methyl-benzamide

HRID 1771788
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HRID 1771788 반응식
[F:1][C:2]1[CH:3]=[C:4]([C:8]2[CH:9]=[C:10]([CH:14]=[C:15]([CH3:17])[CH:16]=2)[C:11]([OH:13])=O)[CH:5]=[CH:6][CH:7]=1.C(Cl)(C(Cl)=O)=O.[NH2:24][C:25]1[C:26]([CH3:33])=[C:27]([OH:32])[CH:28]=[CH:29][C:30]=1[CH3:31].C([O-])(O)=O.[Na+]>C(Cl)Cl.CN(C=O)C.C1COCC1.O>[F:1][C:2]1[CH:3]=[C:4]([C:8]2[CH:9]=[C:10]([CH:14]=[C:15]([CH3:17])[CH:16]=2)[C:11]([NH:24][C:25]2[C:30]([CH3:31])=[CH:29][CH:28]=[C:27]([OH:32])[C:26]=2[CH3:33])=[O:13])[CH:5]=[CH:6][CH:7]=1
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참가 물질

9

반응물 4

HCID 65578Oxalyl chlorideHCID 516892Sodium BicarbonateHCID 141306083-Amino-2,4-dimethylphenolHCID 463145783-(3-Fluorophenyl)-5-methyl-benzoic acid

생성물 1

HCID 894437033-(3-Fluorophenyl)-N-(3-hydroxy-2,6-dimethyl-phenyl)-5-methyl-benzamide수율 70.3%

시약·촉매·용매 4

HCID 6228
Dimethylformamide
촉매
HCID 962Water용매
HCID 6344Dichloromethane용매
HCID 8028Tetrahydrofuran용매2회

실험 절차

To a solution of 3-(3-fluorophenyl)-5-methyl-benzoic acid (300 mg, 1.30 mmol, 1.1 eq) (III(q)) in CH2Cl2 (10 mL) was added (COCl)2 (610 mg, 4.81 mmol, 3.3 eq) and DMF (5 drops). The reaction mixture was stirred at room temperature for 2 h. The resulting mixture was concentrated under reduced pressure to remove the solvent and excess reagent. The residue obtained was dissolved in THF (10 mL) and added dropwise to a mixture of 3-amino-2,4-dimethylphenol (intermediate X(c)) (163 mg, 1.18 mmol, 1.0 eq) and NaHCO3 (612 mg, 7.30 mmol, 5.0 eq) in THF (20 mL) at 0° C. After addition was completed, the reaction mixture was allowed to warm to room temperature and stirred for 1 h. The resulting mixture was poured into water and extracted with EtOAc. The combined organic extracts were washed with water and brine, dried (Na2SO4), filtered, and evaporated in vacuo. The crude product obtained was purified by column chromatography (CH2Cl2: MeOH, 500:1 to 300:1) to give the title compound as a white solid (290 mg, 57%).

후처리

  1. concentrationThe resulting mixture was concentrated under reduced pressure
  2. customto remove the solvent and excess reagent
  3. customThe residue obtained
  4. additionAfter addition
  5. temperatureto warm to room temperature
  6. stirringstirred for 1 h
  7. extractionextracted with EtOAc
  8. washThe combined organic extracts were washed with water and brine
  9. dry with materialdried (Na2SO4)
  10. filtrationfiltered
  11. customevaporated in vacuo
  12. customThe crude product obtained
  13. customwas purified by column chromatography (CH2Cl2: MeOH, 500:1 to 300:1)

출처 및 근거

ORD 기록
ord-2af70e319fdc4809800b807611752005
출처 데이터셋
uspto-grants-2016_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09249085B2

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