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3,5-Dinitrobenzoyl chloride → HCID 21201139、化合物

HRID 1978798
ノート
印刷プレビュー

反応式

HRID 1978798 の反応式
[OH:1][CH2:2][CH2:3][N:4]1[C:8](=[O:9])[CH:7]=[C:6]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[C:5]1=[O:16].O1CCOCC1.C(N(CC)CC)C.[N+:30]([C:33]1[CH:34]=[C:35]([CH:39]=[C:40]([N+:42]([O-:44])=[O:43])[CH:41]=1)[C:36](Cl)=[O:37])([O-:32])=[O:31]>O>[N+:30]([C:33]1[CH:34]=[C:35]([CH:39]=[C:40]([N+:42]([O-:44])=[O:43])[CH:41]=1)[C:36]([O:1][CH2:2][CH2:3][N:4]1[C:8](=[O:9])[CH:7]=[C:6]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[C:5]1=[O:16])=[O:37])([O-:32])=[O:31]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 74323,5-Dinitrobenzoyl chlorideHCID 8471TriethylamineHCID 312751,4-Dioxane2 回HCID 212011151-(2-Hydroxyethyl)-3-phenyl-1H-pyrrole-2,5-dione

生成物 1

HCID 21201139HCID 21201139、化合物収率 29.7%

試薬・触媒・溶媒 1

HCID 962
Water
溶媒

実験手順

In a 11 three-necked flask equipped with a dropping funnel and a stirring means were placed 11.0 g of N-(2-hydroxyethyl)-a-phenylmaleimide and 500 ml of dioxane, and 7.70 ml of triethylamine was added at 0° C. under stirring. A dioxane solution of 11.5 g of 3,5-dinitrobenzoyl chloride was added dropwise thereto at 0° C. and stirring was continued at room temperature overnight. After completion of the reaction, 11 of water was added to the reaction solution and the resulting crystalline substance was collected by filtration. It was recrystallized twice from ethyl acetate to afford 6.10 g of N-(2-(3,5-dinitrobenzoyl)oxyethyl)-α-phenylmaleimide. This compound was subjected to reduction of a nitro group without any further purification. This compound had a melting point of 179.1-180.7° C.

後処理

  1. customIn a 11 three-necked flask equipped with a dropping funnel
  2. additionwas added at 0° C.
  3. stirringat 0° C. and stirring
  4. additionwas added to the reaction solution
  5. filtrationthe resulting crystalline substance was collected by filtration
  6. customIt was recrystallized twice from ethyl acetate

出典と根拠

ORDレコード
ord-d09f997ab8dd4b2eb0fe9e6b4471f8be
出典データセット
uspto-grants-2001_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06238752B1

反応ノート

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