Nitric Acid → HCID 18983889, 화합물

HRID 1440467노트

반응식

HRID 1440467 반응식
[CH2:1]([O:3][C:4]([C:6]1[N:7]=[C:8]2[C:13]([C:14]([O:16][CH2:17][CH3:18])=[O:15])=[CH:12][CH:11]=[CH:10][N:9]2[CH:19]=1)=[O:5])[CH3:2].[N+:20]([O-])([OH:22])=[O:21].[OH-].[Na+]>S(=O)(=O)(O)O>[CH2:1]([O:3][C:4]([C:6]1[N:7]=[C:8]2[C:13]([C:14]([O:16][CH2:17][CH3:18])=[O:15])=[CH:12][CH:11]=[CH:10][N:9]2[C:19]=1[N+:20]([O-:22])=[O:21])=[O:5])[CH3:2]

참가 물질

5

반응물 3

HCID 944Nitric AcidHCID 14798Sodium HydroxideHCID 189838522,8-Diethyl imidazo[1,2-a]pyridine-2,8-dicarboxylate

생성물 1

HCID 18983889HCID 18983889, 화합물수율 53.8%

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매

실험 절차

Ethyl 2-ethoxycarbonylimidazo[1,2-a]pyridine-8-carboxylate (3.8 g, 14.5 m mol) was dissolved in conc. sulfuric acid (10 ml), and to the solution was slowly added 70% nitric acid (1.5 ml) at 10° C. The mixture was stirred at room temperature for 30 minutes, poured into ice water and adjusted to pH 7 by adding 20% sodium hydroxide. The precipitated crystals were filtered to obtain ethyl 2-ethoxycarbonyl-3-nitro-imidazo[1,2-a]pyridine-8-carboxylate (2.4 g, yield 53.8%) as crystals of m.p. 139°-140° C. A solution of the crystals in conc. hydrochloric acid (35 ml) was refluxed for 1.5 hours and cooled to room temperature. The precipitated crystals were collected by filtration and dried to give the object compound (1.2 g, yield 74.3%) of m.p.>300° C.

후처리

  1. customat 10° C
  2. filtrationThe precipitated crystals were filtered

출처 및 근거

ORD 기록
ord-d8d857799f544678a0ac714e1dabf544
출처 데이터셋
uspto-grants-1996_03
특허 번호
US05498774

반응 노트

불러오는 중…