Perchloric Acid → HCID 21998067、化合物

HRID 1977444ノート

反応式

HRID 1977444 の反応式
[O:1]1[CH2:18][CH:2]1[CH2:3][O:4][C:5]1[CH:10]=[CH:9][C:8]([N:11]2[C:15](=[O:16])[CH:14]=[CH:13][C:12]2=[O:17])=[CH:7][CH:6]=1.Cl(O)(=O)(=O)=[O:20].ClCCl.CO>CC(C)=O.O>[OH:20][CH:2]([CH2:18][OH:1])[CH2:3][O:4][C:5]1[CH:6]=[CH:7][C:8]([N:11]2[C:12](=[O:17])[CH:13]=[CH:14][C:15]2=[O:16])=[CH:9][CH:10]=1

参加物

6

反応物 3

HCID 24247Perchloric AcidHCID 21226129Dichloromethane methanolHCID 219980621H-Pyrrole-2,5-dione, 1-[4-(oxiranylmethoxy)phenyl]-

生成物 1

HCID 21998067HCID 21998067、化合物

試薬・触媒・溶媒 2

HCID 180Acetone溶媒HCID 962Water溶媒

実験手順

To a suspension of N-(4-[2,3-epoxypropyl]oxyphenyl)maleimide (200 g, 0.816 mole) in 1360 ml of acetone was added perchloric acid (20 ml) in 660 ml of water. The reaction mixture was refluxed for 2 h, during which the solution became clear yellow (complete conversion on TLC, dichloromethane: methanol 90:10). After cooling, the acetone was removed under reduced pressure. Water was added to the resulting slurry which was stirred for 0.5 h. The solids were filtered off, washed with water and dissolved in THF (tetrahydrofuran). This solution was dried twice over anhydrous sodium sulfate, followed by concentration to dryness.

後処理

  1. temperatureThe reaction mixture was refluxed for 2 h, during which the solution
  2. temperatureAfter cooling
  3. customthe acetone was removed under reduced pressure
  4. additionWater was added to the resulting slurry which
  5. filtrationThe solids were filtered off
  6. washwashed with water
  7. dissolutiondissolved in THF (tetrahydrofuran)
  8. dry with materialThis solution was dried twice over anhydrous sodium sulfate
  9. concentrationfollowed by concentration to dryness

出典と根拠

ORDレコード
ord-0423c2c9f6b54f89a41049d9c0568e20
出典データセット
uspto-grants-2001_05
特許番号
US06232430B1

反応ノート

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