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Water → N,N'-Dibenzyl-3-aminopyrrolidine

HRID 1165569
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HRID 1165569 반응식
[CH2:1]([NH2:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-].O.[OH-].[K+]>O1CCCC1>[CH2:1]([N:8]1[CH2:4][CH2:3][CH:2]([NH:8][CH2:1][C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=2)[CH2:1]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962Water2회HCID 7504BenzylamineHCID 14797Potassium HydroxideHCID 21226445Aluminium lithium hydride

생성물 1

HCID 14098325N,N'-Dibenzyl-3-aminopyrrolidine

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매4회

실험 절차

1,000 g (5.34 mols) of 1-benzyl-Δ3 -pyrroline-2,5-dione are dissolved in 2.5 l of tetrahydrofuran, and 572 g (5.34 mols) of benzylamine are added with stirring at 10° to 20° C. The mixture is left to stand for 24 hours at room temperature, after which 360 g are removed from the resulting solution (3,848 g of total weight) and added to a solution of 38 g (1 mol) of lithium aluminum hydride in 380 ml of absolute dehydrated tetrahydrofuran. The mixture is refluxed for 20 hours, 500 ml of tetrahydrofuran, 38 g of water and 120 ml of tetrahydrofuran, 38 g of 10% strength potassium hydroxide solution and 114 g of water are then sucessively added to the mixture. The salts are filtered off with suction, washed with tetrahydrofuran, the filtrate is concentrated, and the residue is distilled.

후처리

  1. waitThe mixture is left
  2. customafter which 360 g are removed from the resulting solution (3,848 g of total weight)
  3. temperatureThe mixture is refluxed for 20 hours
  4. filtrationThe salts are filtered off with suction
  5. washwashed with tetrahydrofuran
  6. concentrationthe filtrate is concentrated
  7. distillationthe residue is distilled

출처 및 근거

ORD 기록
ord-88a4f23619b44c5baad87a92b773ac16
출처 데이터셋
uspto-grants-1990_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04910319

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