Potassium Iodide → HCID 86754176、化合物

HRID 581066ノート

反応式

HRID 581066 の反応式
BrBr.Br[CH2:4][CH2:5][O:6][C:7]1[C:16]2[O:15][CH2:14][CH2:13][O:12][C:11]=2[CH:10]=[CH:9][CH:8]=1.[C:17]1(=[O:27])[NH:21][C:20](=[O:22])[C:19]2=[CH:23][CH:24]=[CH:25][CH:26]=[C:18]12.[K].[I-].[K+]>CN(C)C=O>[O:12]1[C:11]2[CH:10]=[CH:9][CH:8]=[C:7]([O:6][CH2:5][CH2:4][N:21]3[C:17](=[O:27])[C:18]4[C:19](=[CH:23][CH:24]=[CH:25][CH:26]=4)[C:20]3=[O:22])[C:16]=2[O:15][CH2:14][CH2:13]1

参加物

6

反応物 4

HCID 4875Potassium IodideHCID 24408BromineHCID 27355665-(2-Bromoethoxy)-2,3-dihydro-1,4-benzodioxineHCID 24194345Phthalimide potassium salt

生成物 1

HCID 86754176HCID 86754176、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

Replacement of the bromine of the compound obtained in Step A is carried out in dimethylformamide (10 ml) under an argon atmosphere in the presence of potassium phthalimide (1.5 eq.) catalysed by potassium iodide (0.07 eq.). The reaction mixture is stirred and heated at reflux for 3 hours. The residual and resulting salts are removed by filtration; the product is then precipitated in the cold by the addition of water to the filtrate. The solid formed is filtered and then dried in vacuo in the presence of phosphorus pentoxide.

後処理

  1. temperatureheated
  2. temperatureat reflux for 3 hours
  3. customThe residual and resulting salts
  4. customare removed by filtration
  5. customthe product is then precipitated in the cold by the addition of water to the filtrate
  6. customThe solid formed
  7. filtrationis filtered
  8. dry with materialdried in vacuo in the presence of phosphorus pentoxide

出典と根拠

ORDレコード
ord-c0bd2d2f8cdd4fbd9e58c430d403aea5
出典データセット
uspto-grants-1999_07
特許番号
US05919814

反応ノート

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