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Acetaldehyde → HCID 13504017、化合物

HRID 35525
ノート
印刷プレビュー

反応式

HRID 35525 の反応式
[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
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 3

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

生成物 1

HCID 13504017HCID 13504017、化合物

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 962Water溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-b2cb560d82164e9da8fede7bfd89bc86
出典データセット
uspto-grants-1988_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04767759

反応ノート

読み込み中…

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