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3,5-Dinitrobenzoyl chloride → HCID 21201139, 화합물

HRID 2288945
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HRID 2288945 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]
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참가 물질

6

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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

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온도
0 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-9f7e3b89ebfe4b96a48b1f67443b98c1
출처 데이터셋
uspto-grants-2000_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06090909

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