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

HRID 1771823
ノート
印刷プレビュー

反応式

HRID 1771823 の反応式
[F:1][C:2]1[CH:3]=[C:4]([C:9]2[CH:10]=[C:11]([CH3:19])[C:12]([CH3:18])=[C:13]([CH:17]=2)[C:14]([OH:16])=O)[CH:5]=[C:6]([F:8])[CH:7]=1.C(Cl)(C(Cl)=O)=O.[NH2:26][C:27]1[C:28]([F:35])=[C:29]([OH:34])[CH:30]=[CH:31][C:32]=1[F:33].C([O-])(O)=O.[Na+]>C(Cl)Cl.CN(C=O)C.C1COCC1.O>[F:35][C:28]1[C:29]([OH:34])=[CH:30][CH:31]=[C:32]([F:33])[C:27]=1[NH:26][C:14](=[O:16])[C:13]1[CH:17]=[C:9]([C:4]2[CH:5]=[C:6]([F:8])[CH:7]=[C:2]([F:1])[CH:3]=2)[CH:10]=[C:11]([CH3:19])[C:12]=1[CH3:18]
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 4

HCID 65578Oxalyl chlorideHCID 516892Sodium BicarbonateHCID 227559833-Amino-2,4-difluorophenolHCID 894437345-(3,5-Difluorophenyl)-2,3-dimethyl-benzoic acid

生成物 1

HCID 89443518N-(2,6-Difluoro-3-hydroxy-phenyl)-5-(3,5-difluorophenyl)-2,3-dimethyl-benzamide収率 15.5%

試薬・触媒・溶媒 4

HCID 6228
Dimethylformamide
触媒
HCID 962Water溶媒
HCID 6344Dichloromethane溶媒
HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To a solution of 5-(3,5-difluorophenyl)-2,3-dimethyl-benzoic acid (240 mg, 0.92 mmol, 1.1 eq) in CH2Cl2 (12 mL) was added (COCl)2 (348 mg, 2.75 mmol, 3.3 eq) and DMF (5 drops). The reaction mixture was stirred at room temperature for 1.5 h, then concentrated under reduced pressure to remove the organic solvent and excess reagent. The residue obtained was dissolved in THF (10 mL) and added dropwise to a solution of 3-amino-2,4-difluorophenol (intermediate X(a)) (121 mg, 0.83 mmol, 1.0 eq) and NaHCO3 (386 mg, 4.6 mmol, 5.0 eq) in THF (10 mL) at 0° C. After the addition, the reaction mixture was stirred at room temperature for 1 h. The resulting mixture was diluted with water and extracted with EtOAc. The organic extract was washed with water and brine, dried (Na2SO4), filtered and evaporated in vacuo. The residue was purified by column chromatography (CH2Cl2:MeOH, 500:1 to 200:1) to give the title compound as a yellow solid (50 mg, 15%).

後処理

  1. concentrationconcentrated under reduced pressure
  2. customto remove the organic solvent and excess reagent
  3. customThe residue obtained
  4. additionAfter the addition
  5. stirringthe reaction mixture was stirred at room temperature for 1 h
  6. extractionextracted with EtOAc
  7. extractionThe organic extract
  8. washwas washed with water and brine
  9. dry with materialdried (Na2SO4)
  10. filtrationfiltered
  11. customevaporated in vacuo
  12. customThe residue was purified by column chromatography (CH2Cl2:MeOH, 500:1 to 200:1)

出典と根拠

ORDレコード
ord-18f87f714d2e48e6811e90850c357224
出典データセット
uspto-grants-2016_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09249085B2

反応ノート

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