2-Aminopyridine → HCID 13633211, 화합물

HRID 2118495노트

반응식

HRID 2118495 반응식
C(N1C=CN=C1)(N1C=CN=C1)=O.[N+:13]1([O-:22])[C:14]([C:19]([OH:21])=O)=[CH:15][CH:16]=[CH:17][CH:18]=1.[NH2:23][C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][N:25]=1>CN(C)C=O>[N:25]1[CH:26]=[CH:27][CH:28]=[CH:29][C:24]=1[NH:23][C:19]([C:14]1[N+:13]([O-:22])=[CH:18][CH:17]=[CH:16][CH:15]=1)=[O:21]

참가 물질

5

반응물 3

HCID 104392-AminopyridineHCID 682631,1'-CarbonyldiimidazoleHCID 69986Pyridine-2-carboxylic acid 1-oxide

생성물 1

HCID 13633211HCID 13633211, 화합물수율 0.1%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

1,1'-Carbonyldiimidazole (4.254 g, 26.2 mol) was added to a solution of picolinic acid N-oxide (3.318g, 23.9 mol) in dry dimethylformamide (50 ml). After 4 hours, 2-aminopyridine (2.466 g, 26.2 mol) was added. After 1 hour, the solution was warmed to 100° for 80 minutes and cooled to room temperature. After 18 hours the solution was subjected to evaporation in vacuo to give an oil which slowly crystallised. The solid was recrystallised from EtOH to give the title compound (3.775 g) as needles, m.p. 140°-5°.

후처리

  1. waitAfter 1 hour
  2. temperaturethe solution was warmed to 100° for 80 minutes
  3. customAfter 18 hours the solution was subjected to evaporation in vacuo
  4. customto give an oil which
  5. customslowly crystallised
  6. customThe solid was recrystallised from EtOH

출처 및 근거

ORD 기록
ord-3fe7cfe342a242d3a439e166c0fd66f1
출처 데이터셋
uspto-grants-1987_07
특허 번호
US04678794

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