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Sodium Carbonate → Phthalimide

HRID 846052
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HRID 846052 반응식
FC(F)(F)C1N=C(N2CCNCC2)C=CC=1.BrCC[N:20]1[C:24](=[O:25])[C:23]2=[CH:26][CH:27]=[CH:28][CH:29]=[C:22]2[C:21]1=[O:30].C(=O)([O-])[O-].[Na+].[Na+]>>[C:21]1(=[O:30])[C:22]2[C:23](=[CH:26][CH:27]=[CH:28][CH:29]=2)[C:24](=[O:25])[NH:20]1
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참가 물질

4

반응물 3

HCID 10340Sodium CarbonateHCID 113251H-Isoindole-1,3(2H)-dione, 2-(2-bromoethyl)-HCID 114247401-[6-(Trifluoromethyl)pyridin-2-yl]piperazine

생성물 1

HCID 6809Phthalimide수율 33%

실험 절차

A mixture of 69.3 g of 1-[6-(trifluoromethyl) -2-pyridinyl]piperazine, and 129.6 g of N-(2-bromo-ethyl)phthalimide and 57.2 g of sodium carbonate is heated at reflux for 23 hours. The resulting precipitate is filtered off and the ethanol evaporated. The concentrate is dissolved in dichloromethane, washed with water, dried over magnesium sulfate, and evaporated. The resulting precipitate is recrystallized from isopropanol to give 39.5 g of 2-μ-[4-[6-(trifluoromethyl)-2-pyridinyl]-1-piperazinyl]ethyl]-1H-isoindole-1,3-dione (yield 33%).

후처리

  1. temperatureis heated
  2. temperatureat reflux for 23 hours
  3. filtrationThe resulting precipitate is filtered off
  4. customthe ethanol evaporated
  5. dissolutionThe concentrate is dissolved in dichloromethane
  6. washwashed with water
  7. dry with materialdried over magnesium sulfate
  8. customevaporated
  9. customThe resulting precipitate is recrystallized from isopropanol

출처 및 근거

ORD 기록
ord-bc13360904ee4f8bbecca02d45dd1f82
출처 데이터셋
uspto-grants-1992_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05135931

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