乙醚 → 6-(Acetylamino)-4-methyl-3-pyridinediazonium tetrafluoroborate

HRID 1828542

反应方程式

HRID 1828542 反应方程式
[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]

参与物

5

反应物 4

HCID 3283乙醚HCID 28118氟硼酸HCID 220635734-甲基-2-乙酰氨基-5-氨基吡啶2 次HCID 23668193亚硝酸钠

产物 1

HCID 220636686-(Acetylamino)-4-methyl-3-pyridinediazonium tetrafluoroborate

反应条件

温度
-10 °C

实验过程

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).

后处理

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

来源与证据

ORD记录
ord-cbb21bec42474f60a019da7ee26d175a
来源数据集
uspto-grants-2006_06
专利号
US07056917B2

关联笔记

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