Diethyl Ether → 6-(Acetylamino)-4-methyl-3-pyridinediazonium tetrafluoroborate

HRID 1828542

반응식

HRID 1828542 반응식
[NH2:1][C:2]1[C:3]([CH3:12])=[CH:4][C:5]([NH:8][C:9](=[O:11])[CH3:10])=[N:6][CH:7]=1.[N:13]([O-])=O.[Na+].C(OCC)C.[F:22][B-:23]([F:26])([F:25])[F:24].[H+]>>[F:22][B-:23]([F:26])([F:25])[F:24].[C:9]([NH:8][C:5]1[N:6]=[CH:7][C:2]([N+:1]#[N:13])=[C:3]([CH3:12])[CH:4]=1)(=[O:11])[CH3:10]

참가 물질

5

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온도
-10 °C

실험 절차

The N1-(5-amino-4-methyl-2-pyridyl)acetamide (8.00 g, 48.4 mmol) obtained in (B) was dissolved in tetrafluoroboric acid (160 ml) and slowly added dropwise with an aqueous solution (40 ml) of sodium nitrite (3.51 g, 50.8 mmol) at −20° C. under nitrogen atmosphere. The reaction mixture was further stirred at −10° C. for 1 hour and added with diethyl ether (800 ml), and the deposited white solid was collected by filtration and washed with diethyl ether to obtain the title compound (14.7 g, quantitative).

후처리

  1. filtrationthe deposited white solid was collected by filtration
  2. washwashed with diethyl ether

출처 및 근거

ORD 기록
ord-cbb21bec42474f60a019da7ee26d175a
출처 데이터셋
uspto-grants-2006_06
특허 번호
US07056917B2

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