Ethyl Acetate → HCID 12800846、化合物

HRID 1679185ノート

反応式

HRID 1679185 の反応式
Br.[NH2:2][CH2:3][C:4]([O:6][CH2:7][C:8]1[CH:13]=[CH:12][C:11]([N+:14]([O-:16])=[O:15])=[CH:10][CH:9]=1)=[O:5].CCOC(C)=O.C([O-])([O-])=O.[K+].[K+]>O>[NH2:2][CH2:3][C:4]([O:6][CH2:7][C:8]1[CH:13]=[CH:12][C:11]([N+:14]([O-:16])=[O:15])=[CH:10][CH:9]=1)=[O:5]

参加物

5

反応物 3

HCID 8857Ethyl AcetateHCID 11430Potassium CarbonateHCID 20516785p-Nitrobenzyl glycinate hydrobromide

生成物 1

HCID 12800846HCID 12800846、化合物収率 98%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

p-Nitrobenzyl glycinate hydrobromide (7.15 g., 24.6 mMol) is suspended in H2O (15 ml.) and the mixture is layered with EtOAc (40 ml.). The mixture is cooled in ice and stirred while cold, saturated aqueous K2CO3 (6 ml.) is added. The layers are separated and the aqueous portion is extracted with more EtOAc (3 × 15 ml.). The combined EtOAc solution is dried over Na2SO4, filtered and evaporated in vacuo to provide p-nitrobenzyl glycinate (5.05 g., 24.0 mMol, 98% yield) as an off-white solid.

後処理

  1. temperatureThe mixture is cooled in ice
  2. additionis added
  3. customThe layers are separated
  4. extractionthe aqueous portion is extracted with more EtOAc (3 × 15 ml.)
  5. dry with materialThe combined EtOAc solution is dried over Na2SO4
  6. filtrationfiltered
  7. customevaporated in vacuo

出典と根拠

ORDレコード
ord-85288bfa059f40b0938c92bc24766210
出典データセット
uspto-grants-1978_03
特許番号
US04079179

反応ノート

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