Sodium ethoxide → 4-Oxo-pyrrolidine-1,3-dicarboxylic acid diethyl ester

HRID 659045ノート

反応式

HRID 659045 の反応式
[CH2:1]([O:3][C:4]([N:6]([CH2:14][C:15]([O:17]CC)=O)[CH2:7][CH2:8][C:9]([O:11][CH2:12][CH3:13])=[O:10])=[O:5])[CH3:2].CC[O-].[Na+]>CCO>[O:17]=[C:15]1[CH2:14][N:6]([C:4]([O:3][CH2:1][CH3:2])=[O:5])[CH2:7][CH:8]1[C:9]([O:11][CH2:12][CH3:13])=[O:10]

参加物

4

反応物 2

HCID 2723922Sodium ethoxideHCID 4381617ethyl 3-[ethoxycarbonyl-(2-ethoxy-2-oxoethyl)amino]propanoate

生成物 1

HCID 2763144-Oxo-pyrrolidine-1,3-dicarboxylic acid diethyl ester

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
80 °C

実験手順

Intermediate (e) (18.0 g, 65.2 mmol) was added to an ice bath cooled solution of NaOEt (32.6 mL) (21% by weight in EtOH) in absolute EtOH (41.7 mL) under a nitrogen atmosphere. The ice bath was removed and the mixture was heated at 80° C. for about 12 h until the condensation was complete as observed by TLC. The mixture was poured onto ice/water and extracted into EtOAc. The solvent was dried with Na2SO4, filtered, and evaporated to afford crude intermediate (f) as an off white solid (14.05 g) which was carried on without purification.

後処理

  1. customThe ice bath was removed
  2. additionThe mixture was poured onto ice/water
  3. extractionextracted into EtOAc
  4. dry with materialThe solvent was dried with Na2SO4
  5. filtrationfiltered
  6. customevaporated

出典と根拠

ORDレコード
ord-cdf601ddefbc45f5a832363300a87067
出典データセット
uspto-grants-2011_12
特許番号
US08080556B2

反応ノート

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