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

HRID 2288945
ノート
印刷プレビュー

反応式

HRID 2288945 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]
参加物反応条件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

反応条件

温度
0 °C

実験手順

A three neck flask of 1 l equipped with a dropping funnel and a stirrer was charged with 11.1 g of N-(2-hydroxyethyl)-α-phenylmaleimide and 500 ml of dioxane, and 7.70 ml of triethylamine was added while stirring at 0° C. A dioxane solution of 11.5 g of 3,5-dinitrobenzoyl chloride was dropwise added thereto at 0° C., and the mixture was stirred at a room temperature all the night through. After finishing the reaction, the reaction solution was added to 1 l of water to filter the resulting crystal. This was recrystallized in ethyl acetate twice to obtain 6.10 g of N-(2-(3, 5-dinitrobenzoyl) oxyethyl)-α-phenylmaleimide. This compound was subjected to reduction of a nitro group without refining furthermore. This compound had a melting point of 179.1 to 180.7° C.

後処理

  1. customA three neck flask of 1 l equipped with a dropping funnel and a stirrer
  2. additionwas added
  3. stirringat 0° C., and the mixture was stirred at a room temperature all the night through
  4. customthe reaction
  5. filtrationto filter the resulting crystal
  6. customThis was recrystallized in ethyl acetate twice

出典と根拠

ORDレコード
ord-9f7e3b89ebfe4b96a48b1f67443b98c1
出典データセット
uspto-grants-2000_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06090909

反応ノート

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