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Hydrogen Bromide → 1,2,3,4,5,6-Hexahydropyrrolo[3,4-c]pyrrole dihydrobromide

HRID 1534644
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HRID 1534644 반응식
C1(O)C=CC=CC=1.C1(C)C=CC(S([N:17]2[CH2:24][C:23]3[CH2:22][N:21](S(C4C=CC(C)=CC=4)(=O)=O)[CH2:20][C:19]=3[CH2:18]2)(=O)=O)=CC=1.[BrH:36]>>[BrH:36].[BrH:36].[C:19]12[CH2:20][NH:21][CH2:22][C:23]=1[CH2:24][NH:17][CH2:18]2
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참가 물질

4

반응물 3

HCID 260Hydrogen BromideHCID 996PhenolHCID 151922522,5-Ditosyl-1,2,3,4,5,6-hexahydropyrrolo[3,4-c]pyrrole

생성물 1

HCID 232828491,2,3,4,5,6-Hexahydropyrrolo[3,4-c]pyrrole dihydrobromide

실험 절차

60 ml of 48% hydrobromic acid and 7 g of phenol were added to 10.8 g 3,7bis-p-toluenesulfonyl-3,7-diazabicyclo[3.3.0]oct-1-(5)-ene, prepared in Preparation 1. The mixture was refluxed for 4 hours and cooled to room temperature. The aqueous phase was separated by adding 100 ml of chloroform and 50 ml of water. The aqueous phase was washed with chloroform (100 ml×4) and decolorized with active carbon. The aqueous phase was concentrated under vacuum and the remained solid was washed with 1:1 methanol-ethyl ether solvent. 5 g of the title compound was obtained as white solid (yield 71%).

후처리

  1. customprepared in Preparation 1
  2. temperatureThe mixture was refluxed for 4 hours
  3. customThe aqueous phase was separated
  4. additionby adding 100 ml of chloroform and 50 ml of water
  5. washThe aqueous phase was washed with chloroform (100 ml×4)
  6. concentrationThe aqueous phase was concentrated under vacuum
  7. washthe remained solid was washed with 1:1 methanol-ethyl ether solvent

출처 및 근거

ORD 기록
ord-87877351dbab458e9a9e51949b849df4
출처 데이터셋
uspto-grants-1992_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05089621

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