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Water → 5-Benzyl-1-methyl-octahydropyrrolo[3,4-b]pyrrole

HRID 36666
ノート
印刷プレビュー

反応式

HRID 36666 の反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH2:7]([N:14]1[C:21](=O)[CH:20]2[CH:16]([N:17]([CH3:23])[CH2:18][CH2:19]2)[C:15]1=O)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.O.[OH-].[K+]>O1CCCC1>[CH2:7]([N:14]1[CH2:21][CH:20]2[CH:16]([N:17]([CH3:23])[CH2:18][CH2:19]2)[CH2:15]1)[C:8]1[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962Water2 回HCID 14797Potassium HydroxideHCID 15069999HCID 15069999、化合物HCID 21226445Aluminium lithium hydride

生成物 1

HCID 150700005-Benzyl-1-methyl-octahydropyrrolo[3,4-b]pyrrole

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

1.52 g (40 mmol) of lithium aluminum hydride are initially introduced into 30 ml of anhydrous tetrahydrofuran, and 4.9 g (20 mmol) of 5-benzyl-4,6-dioxo-1-methyl-octahydropyrrolo[3,4-b]pyrrole are added dropwise as a solution in 15 ml of anhydrous tetrahydrofuran. The mixture is then subsequently stirred at the boiling point for 3 hours. 1.5 ml of water, 1.5 ml of 15% strength potassium hydroxide solution and 4.5 ml of water are added dropwise in succession to the batch and the precipitate is then filtered off with suction and washed with tetrahydrofuran. The filtrate is concentrated on a rotary evaporator and the residue is distilled. 3.1 g (72% of theory) of a colorless distillate of boiling point 80° C./0.07 mbar are obtained.

後処理

  1. filtrationthe precipitate is then filtered off with suction
  2. washwashed with tetrahydrofuran
  3. concentrationThe filtrate is concentrated on a rotary evaporator
  4. distillationthe residue is distilled
  5. custom3.1 g (72% of theory) of a colorless distillate of boiling point 80° C./0.07 mbar are obtained

出典と根拠

ORDレコード
ord-1d1644f157d4411987607b8080c1e3eb
出典データセット
uspto-grants-1995_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05416096

反応ノート

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