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Potassium Hydroxide → HCID 13363165、化合物

HRID 1979986
ノート
印刷プレビュー

反応式

HRID 1979986 の反応式
[OH-].[K+].[CH2:3]([O:5][C:6]([C@H:8]1[CH2:12][CH2:11][C@H:10]([C:13]([O:15]CC)=[O:14])[N:9]1[CH2:18][C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)=[O:7])[CH3:4]>C(O)C>[CH2:3]([O:5][C:6]([CH:8]1[CH2:12][CH2:11][CH:10]([C:13]([OH:15])=[O:14])[N:9]1[CH2:18][C:19]1[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=1)=[O:7])[CH3:4]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 14797Potassium HydroxideHCID 6932551diethyl (2R,5R)-1-benzylpyrrolidine-2,5-dicarboxylate

生成物 1

HCID 13363165HCID 13363165、化合物収率 65%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

Potassium hydroxide (6.7 g, 0.1 m) in ethanol (180 ml) was slowly added to a solution of trans-1-benzyl-2,5-pyrrolidine dicarboxylic acid diethyl ester in ethanol (300 ml) at room temperature. This was stirred for 36 hours. The solvent was evaporated off and the residue dissolved in water. The pH of the solution was adjusted to 8 with dilute hydrochloric acid and the solution extracted with hexane to remove the unreacted amino diester. The aqueous solution was adjusted to a pH of 5.3 and was then extracted with diethyl ether. The combined extracts were washed with brine, dried over anhydrous sodium sulfate and concentrated, giving 18.3 g (65%) of the title compound as an oil.

後処理

  1. customThe solvent was evaporated off
  2. dissolutionthe residue dissolved in water
  3. extractionthe solution extracted with hexane
  4. customto remove the unreacted amino diester
  5. extractionwas then extracted with diethyl ether
  6. washThe combined extracts were washed with brine
  7. dry with materialdried over anhydrous sodium sulfate
  8. concentrationconcentrated

出典と根拠

ORDレコード
ord-d71a9550c04647a692af904498594f4c
出典データセット
uspto-grants-1984_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04483991

反応ノート

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