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

HRID 1534809
ノート
印刷プレビュー

反応式

HRID 1534809 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 3

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

生成物 1

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

実験手順

60 ml of 48% hydrobromic acid and 7 g of phenol were added to 10.8 g 3,7-bis-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%).

後処理

  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

出典と根拠

ORDレコード
ord-9979fa4531894658a16206b26a561fe7
出典データセット
uspto-grants-1992_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05091384

反応ノート

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