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3,5-Dinitrobenzoyl chloride → HCID 21201139, 화합물

HRID 1978798
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HRID 1978798 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 74323,5-Dinitrobenzoyl chlorideHCID 8471TriethylamineHCID 312751,4-Dioxane2회HCID 212011151-(2-Hydroxyethyl)-3-phenyl-1H-pyrrole-2,5-dione

생성물 1

HCID 21201139HCID 21201139, 화합물수율 29.7%

시약·촉매·용매 1

HCID 962
Water
용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d09f997ab8dd4b2eb0fe9e6b4471f8be
출처 데이터셋
uspto-grants-2001_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06238752B1

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