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Ethyl Acetate → N-Methyl-3-[4-(4-nitrobenzyl)-2,5-dioxoimidazolidinylmethyl]benzamide

HRID 483369
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HRID 483369 반응식
[N+:1]([C:4]1[CH:17]=[CH:16][C:7]([CH2:8][CH:9]2[C:13](=[O:14])[NH:12][C:11](=[O:15])[NH:10]2)=[CH:6][CH:5]=1)([O-:3])=[O:2].Cl[CH2:19][C:20]1[CH:21]=[C:22]([CH:27]=[CH:28][CH:29]=1)[C:23]([NH:25][CH3:26])=[O:24].C([O-])([O-])=O.[K+].[K+].C(OCC)(=O)C>CN(C=O)C>[CH3:26][NH:25][C:23](=[O:24])[C:22]1[CH:27]=[CH:28][CH:29]=[C:20]([CH2:19][N:12]2[C:13](=[O:14])[CH:9]([CH2:8][C:7]3[CH:16]=[CH:17][C:4]([N+:1]([O-:3])=[O:2])=[CH:5][CH:6]=3)[NH:10][C:11]2=[O:15])[CH:21]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 8857Ethyl AcetateHCID 11430Potassium CarbonateHCID 104665795-[(4-Nitrophenyl)methyl]imidazolidine-2,4-dioneHCID 226602083-(chloromethyl)-N-methylbenzamide

생성물 1

HCID 10068456N-Methyl-3-[4-(4-nitrobenzyl)-2,5-dioxoimidazolidinylmethyl]benzamide수율 69.2%

시약·촉매·용매 1

HCID 6228
Dimethylformamide
용매

실험 절차

The product from step (a) (4.0 g), the product from step (b) (3.3 g) and anhy. K2CO3 (2.55 g) were taken up in DMF (25 ml) and stirred at room temperature for 60 hours. The mixture was poured with vigorous stirring into ice-water (175 ml) to give an oily precipitate. Ethyl acetate was added and stirring continued for 1 hour to solidify the precipitate. The latter was filtered off, washed with water, ethyl acetate and ether, and dried to give the desired product as a peach-coloured solid (4.5 g).

후처리

  1. additionThe mixture was poured
  2. customto give an oily precipitate
  3. stirringstirring
  4. waitcontinued for 1 hour
  5. filtrationThe latter was filtered off
  6. washwashed with water, ethyl acetate and ether
  7. customdried

출처 및 근거

ORD 기록
ord-492dce69b7e9401193ac8693905e0858
출처 데이터셋
uspto-grants-1993_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05225431

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