2-Amino-3,4-diethoxycarbonyl-6-phenylpyridine hydrochloride → 3,4-Diethoxycarbonyl-6-phenyl-2-pyridone

HRID 37466ノート

反応式

HRID 37466 の反応式
Cl.N[C:3]1[C:8]([C:9]([O:11][CH2:12][CH3:13])=[O:10])=[C:7]([C:14]([O:16][CH2:17][CH3:18])=[O:15])[CH:6]=[C:5]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[N:4]=1.N([O-])=[O:26].[Na+]>Cl.O1CCOCC1.O>[CH2:12]([O:11][C:9]([C:8]1[C:3](=[O:26])[NH:4][C:5]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)=[CH:6][C:7]=1[C:14]([O:16][CH2:17][CH3:18])=[O:15])=[O:10])[CH3:13]

参加物

6

反応物 2

HCID 199356132-Amino-3,4-diethoxycarbonyl-6-phenylpyridine hydrochlorideHCID 23668193Sodium Nitrite

生成物 1

HCID 199356223,4-Diethoxycarbonyl-6-phenyl-2-pyridone

試薬・触媒・溶媒 3

HCID 313Hydrochloric Acid溶媒HCID 962Water溶媒HCID 312751,4-Dioxane溶媒

実験手順

In a mixture of 90 ml of 2% hydrochloric acid and 60 ml of dioxane was dissolved 3.50 g (10 mmol) of 2-amino-3,4-diethoxycarbonyl-6-phenylpyridine hydrochloride. A solution of 0.83 g (1.2 eq.) of sodium nitrite dissolved in 3 ml of water was added dropwise thereto. The mixture was stirred at room temperature for 4 hours and left standing overnight. The solvent was distilled off. The resulting crystals were collected by filtration with water. The crystals were recrystallized from ethanol, to give pale yellow prisms.

後処理

  1. additionwas added dropwise
  2. waitleft
  3. waitstanding overnight
  4. distillationThe solvent was distilled off
  5. filtrationThe resulting crystals were collected by filtration with water
  6. customThe crystals were recrystallized from ethanol
  7. customto give pale yellow prisms

出典と根拠

ORDレコード
ord-3ba45d3f0a9040be8c9e7621a06f83d8
出典データセット
uspto-grants-1995_05
特許番号
US05420275

反応ノート

読み込み中…