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

HRID 37466노트

반응식

HRID 37466 반응식
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]

참가 물질

6

반응물 2

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

생성물 1

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

시약·촉매·용매 3

HCID 313Hydrochloric Acid용매HCID 962Water용매HCID 312751,4-Dioxane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-3ba45d3f0a9040be8c9e7621a06f83d8
출처 데이터셋
uspto-grants-1995_05
특허 번호
US05420275

반응 노트

불러오는 중…