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Dimethylformamide → N-(2,6-Difluoro-3-hydroxy-phenyl)-5-(3,4-difluorophenyl)-2,3-dimethyl-benzamide

HRID 1771818
ノート
印刷プレビュー

反応式

HRID 1771818 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]=[CH:6][C:7]=1[F:8].C(Cl)(C(Cl)=O)=O.CN(C=O)C.[NH2:31][C:32]1[C:33]([F:40])=[C:34]([OH:39])[CH:35]=[CH:36][C:37]=1[F:38].C([O-])(O)=O.[Na+]>C(Cl)Cl.C1COCC1.O>[F:40][C:33]1[C:34]([OH:39])=[CH:35][CH:36]=[C:37]([F:38])[C:32]=1[NH:31][C:14](=[O:16])[C:13]1[CH:17]=[C:9]([C:4]2[CH:5]=[CH:6][C:7]([F:8])=[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 5

HCID 6228DimethylformamideHCID 65578Oxalyl chlorideHCID 516892Sodium BicarbonateHCID 227559833-Amino-2,4-difluorophenolHCID 894452845-(3,4-Difluorophenyl)-2,3-dimethyl-benzoic acid

生成物 1

HCID 89443829N-(2,6-Difluoro-3-hydroxy-phenyl)-5-(3,4-difluorophenyl)-2,3-dimethyl-benzamide
収率 19%

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 6344Dichloromethane溶媒HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To a solution of 5-(3,4-difluorophenyl)-2,3-dimethyl-benzoic acid (395 mg, 1.51 mmol, 1.1 eq) in CH2Cl2 (5 mL) was added (COCl)2 (521.6 mg, 4.11 mmol, 3.0 eq) dropwise at 0° C. DMF (10 mg, 0.14 mmol, 0.1 eq) was added and 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 (4 mL) and added dropwise to a mixture of 3-amino-2,4-difluoro-phenol (intermediate X(a)) (198 mg, 1.37 mmol, 1.0 eq) and NaHCO3 (575 mg, 6.85 mmol, 5.0 eq) in THF (4 mL) at 0° C. After addition was completed the reaction mixture was stirred at room temperature for 30 min. Water was added and the aqueous layer extracted with EtOAc. The combined organic extracts were washed with saturated NaHCO3, water and brinc, dried (Na2SO4), filtered and evaporated in vacuo. The residue was purified by column chromatography (petroleum ether:EtOAc, 10:1 to 4:1) to give the title compound as a white solid (100 mg, 19%).

後処理

  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. stirringwas stirred at room temperature for 30 min
  6. extractionthe aqueous layer extracted with EtOAc
  7. washThe combined organic extracts were washed with saturated NaHCO3, water and brinc
  8. dry with materialdried (Na2SO4)
  9. filtrationfiltered
  10. customevaporated in vacuo
  11. customThe residue was purified by column chromatography (petroleum ether:EtOAc, 10:1 to 4:1)

出典と根拠

ORDレコード
ord-62727e5711b943d29c9d8aa54cd9f545
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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