Acetic Anhydride → Methyl 4-(acetylamino)pyridine-3-carboxylate

HRID 539941

反応式

HRID 539941 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][N:5]=[CH:4][C:3]=1[C:8]([O:10][CH3:11])=[O:9].[C:12](OC(=O)C)(=[O:14])[CH3:13]>O1CCOCC1>[C:12]([NH:1][C:2]1[CH:7]=[CH:6][N:5]=[CH:4][C:3]=1[C:8]([O:10][CH3:11])=[O:9])(=[O:14])[CH3:13]

参加物

4

反応物 2

HCID 7918Acetic AnhydrideHCID 592353Methyl 4-aminopyridine-3-carboxylate

生成物 1

HCID 66524315Methyl 4-(acetylamino)pyridine-3-carboxylate収率 42.9%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

A mixture of methyl 4-aminopyridine-3-carboxylate (100 g, 0.6 mol) and acetic anhydride (240 g, 2.4 mol) in anhydrous 1,4-dioxane (1.2 L) was stirred at room temperature overnight. The reaction mixture was concentrated in vacuo and diluted with water (800 mL). The mixture was neutralized with a saturated aqueous solution of sodium bicarbonate to pH 7. The formed solid was collected by filtration and dried in vacuo to afford 50 g of methyl 4-(acetylamino)pyridine-3-carboxylate as a white solid.

後処理

  1. concentrationThe reaction mixture was concentrated in vacuo
  2. additiondiluted with water (800 mL)
  3. filtrationThe formed solid was collected by filtration
  4. customdried in vacuo

出典と根拠

ORDレコード
ord-da271d1338104b47a3d098c5128eb4f3
出典データセット
uspto-grants-2014_10
特許番号
US08871756B2

関連ノート

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