Hydrogen Peroxide → 2-(4-chlorophenyl)-4,4a,5,6-tetrahydrothieno[2',3':2,3]thiepino[4,5-c]pyridazin-3(2H)-one 7-oxide

HRID 1681839ノート

反応式

HRID 1681839 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[C:13](=[O:14])[CH2:12][CH:11]3[CH2:15][CH2:16][S:17][C:18]4[S:22][CH:21]=[CH:20][C:19]=4[C:10]3=[N:9]2)=[CH:4][CH:3]=1.[OH:23]O>C(O)(=O)C>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[C:13](=[O:14])[CH2:12][CH:11]3[CH2:15][CH2:16][S:17](=[O:23])[C:18]4[S:22][CH:21]=[CH:20][C:19]=4[C:10]3=[N:9]2)=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 784Hydrogen Peroxide3 回HCID 106414982-(4-chlorophenyl)-4,4a,5,6-tetrahydrothieno[2',3':2,3]thiepino[4,5-c]pyridazin-3(2H)-one

生成物 1

HCID 190167982-(4-chlorophenyl)-4,4a,5,6-tetrahydrothieno[2',3':2,3]thiepino[4,5-c]pyridazin-3(2H)-one 7-oxide

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

To a solution of 5.4 g of 2-(4-chlorophenyl)-4,4a,5,6-tetrahydrothieno[2',3':2,3]thiepino[4,5-c]pyridazin-3(2H)-one in 60 ml of acetic acid is added 3.5 ml of 30% aqueous hydrogen peroxide solution under ice-cooling and stirred at the same temperature for 3 hours. Furthermore, to the solution is added 2 ml of 30% aqueous hydrogen peroxide solution and stirred for 2 hours. To the solution is additionally added 2 ml of aqueous 30% hydrogen peroxide solution, stirred for 2 hours and the mixture is poured into ice-cold water. The mixture is extracted with chloroform three times, the extract is washed with water and saline solution and dried over magnesium sulfate. The chloroform is distilled off to give 7 g of 2-(4-chlorophenyl)-4,4a,5,6-tetrahydrothieno[2',3':2,3]thiepino[4,5-c]pyridazin-3(2H)-one 7-oxide as pale brawn oil.

後処理

  1. temperaturecooling
  2. stirringstirred for 2 hours
  3. stirringstirred for 2 hours
  4. additionthe mixture is poured into ice-cold water
  5. extractionThe mixture is extracted with chloroform three times
  6. washthe extract is washed with water and saline solution
  7. dry with materialdried over magnesium sulfate
  8. distillationThe chloroform is distilled off

出典と根拠

ORDレコード
ord-013b8f0409234deba244e2339a02aab8
出典データセット
uspto-grants-1992_12
特許番号
US05175162

反応ノート

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