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Acetaldehyde → HCID 13504017, 화합물

HRID 35525
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HRID 35525 반응식
[CH2:1]([N:8]1[CH2:12][CH:11](N)[CH:10](C)[C:9]1=[O:15])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH:16](=O)[CH3:17].Cl>[Pd].O>[CH2:1]([N:8]1[CH2:12][CH:11]([CH2:9][N:8]([CH2:16][CH3:17])[CH2:1][CH3:2])[CH2:10][C:9]1=[O:15])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 177AcetaldehydeHCID 313Hydrochloric AcidHCID 19354255(-)-1-Benzyl-4-amino-methyl-pyrrolidin-2-one

생성물 1

HCID 13504017HCID 13504017, 화합물

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 962Water용매

실험 절차

A mixture of 11.5 g (0.056 mol) of (-)-1-benzyl-4-amino-methyl-pyrrolidin-2-one, 130 ml of water, 13 g of acetaldehyde, 5.8 ml of concentrated hydrochloric acid and 6.5 g of 20% palladium-on-charcoal was hydrogenated for 51/4 hours at 5 bar and at 25° C. The reaction mixture was filtered, the filtrate was evaporated, the residue was taken up in 30 ml of water, and the solution was extracted with methylene chloride. The aqueous hydrochloric acid solution was made alkaline and then extracted with methylene chloride. By distillation of the combined extracts in a bulbed tube, 11.2 g (76.4% of theory) of the title compound were obtained, αD =-9.4 (c =1.0; :ethanol).

후처리

  1. custom4 hours
  2. customat 25° C
  3. filtrationThe reaction mixture was filtered
  4. customthe filtrate was evaporated
  5. extractionthe solution was extracted with methylene chloride
  6. extractionextracted with methylene chloride
  7. distillationBy distillation of the combined extracts in a bulbed tube

출처 및 근거

ORD 기록
ord-b2cb560d82164e9da8fede7bfd89bc86
출처 데이터셋
uspto-grants-1988_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04767759

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