Potassium Iodide → HCID 86752041、化合物

HRID 861984ノート

反応式

HRID 861984 の反応式
Br[CH2:2][C:3]1[CH:8]=[CH:7][N:6]=[C:5]([N:9]2[C:17](=[O:18])[C:16]3[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=3)[C:10]2=[O:19])[CH:4]=1.[P:20]([O:27]CC)([O:24][CH2:25][CH3:26])[O:21][CH2:22][CH3:23].[I-].[K+]>CCC(C)=O>[O:19]=[C:10]1[C:11]2[C:16](=[CH:15][CH:14]=[CH:13][CH:12]=2)[C:17](=[O:18])[N:9]1[C:5]1[CH:4]=[C:3]([CH2:2][P:20](=[O:27])([O:24][CH2:25][CH3:26])[O:21][CH2:22][CH3:23])[CH:8]=[CH:7][N:6]=1

参加物

5

反応物 3

HCID 4875Potassium IodideHCID 31215Triethyl phosphiteHCID 197011582-(4-(Bromomethyl)pyridin-2-YL)isoindoline-1,3-dione

生成物 1

HCID 86752041HCID 86752041、化合物

試薬・触媒・溶媒 1

HCID 6569Methyl Ethyl Ketone溶媒

実験手順

The product from Example 14, triethyl phosphite (7.66 g, 46 mmol) and a catalytic amount of potassium iodide were placed in a flask containing MEK (500 mL) under a N2 atmosphere. The reaction was heated to reflux for 11 h. After cooling to room temperature, the solid was filtered from the reaction mixture, and the filtrate stripped in vacuo. Aqueous K2 CO3 was added to the residue, and the product extracted with EtOAc. The extract was dried (MgSO4), filtered and stripped of all solvent in vacuo to produce the crude product which was purified by flash chromatography (97/3 CHCl3 /EtOH).

後処理

  1. temperatureThe reaction was heated
  2. temperatureto reflux for 11 h
  3. filtrationthe solid was filtered from the reaction mixture
  4. additionAqueous K2 CO3 was added to the residue
  5. extractionthe product extracted with EtOAc
  6. dry with materialThe extract was dried (MgSO4)
  7. filtrationfiltered

出典と根拠

ORDレコード
ord-aa0c6027c20848e992cb3e23d776193c
出典データセット
uspto-grants-1998_02
特許番号
US05716964

反応ノート

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