Hydrochloric Acid → Diethyl 5-amino-1,6-dihydro-6-oxo-2,3-pyridinedicarboxylate

HRID 742211

反応式

HRID 742211 の反応式
Cl.C([NH:5][C:6]1[C:11](=[O:12])[NH:10][C:9]([C:13]([O:15][CH2:16][CH3:17])=[O:14])=[C:8]([C:18]([O:20][CH2:21][CH3:22])=[O:19])[CH:7]=1)(=O)C>C(O)C>[NH2:5][C:6]1[C:11](=[O:12])[NH:10][C:9]([C:13]([O:15][CH2:16][CH3:17])=[O:14])=[C:8]([C:18]([O:20][CH2:21][CH3:22])=[O:19])[CH:7]=1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 19958266Diethyl 5-acetamido-1,6-dihydro-6-oxo-2,3-pyridinedicarboxylate

生成物 1

HCID 19958246Diethyl 5-amino-1,6-dihydro-6-oxo-2,3-pyridinedicarboxylate

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Hydrogen chloride gas is bubbled into a solution of diethyl 5-acetamido-1,6-dihydro-6-oxo-2,3-pyridinedicarboxylate (5.2 g, 0.018 mol) dissolved in absolute ethanol (400 mL) until the solution is saturated at 20° C. The reaction is stirred at room temperature overnight and is then concentrated in vacuo. The resulting residue is dissolved in water, neutralized with solid sodium bicarbonate, and extracted into methylene chloride. The combined organic extracts are dried over anhydrous sodium sulfate, filtered and concentrated in vacuo to give diethyl 5-amino-1,6-dihydro-6-oxo-2,3-pyridinedicarboxylate as a yellow solid in quantitative yield.

後処理

  1. customis saturated at 20° C
  2. concentrationis then concentrated in vacuo
  3. dissolutionThe resulting residue is dissolved in water
  4. extractionextracted into methylene chloride
  5. dry with materialThe combined organic extracts are dried over anhydrous sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-4d4978ae0cb74b71a9d91a619b091b76
出典データセット
uspto-grants-1996_09
特許番号
US05554579

関連ノート

読み込み中…