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

HRID 974899
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HRID 974899 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962Water2회HCID 14797Potassium HydroxideHCID 15069999HCID 15069999, 화합물HCID 21226445Aluminium lithium hydride

생성물 1

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-b98552a8fb76487fb86117a6a17acd31
출처 데이터셋
uspto-grants-1997_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05607942

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