2-Pyrazinecarbonitrile, 3-azido-6-fluoro- → HCID 22662784，化合物

HRID 392347

反应方程式

HRID 392347 反应方程式
[N:1]([C:4]1[C:5]([C:11]#[N:12])=[N:6][C:7]([F:10])=[CH:8][N:9]=1)=[N+]=[N-].[H][H]>CO.C(=O)([O-])[O-].[Ca+2].[Pd+2].C(=O)([O-])[O-]>[NH2:1][C:4]1[C:5]([C:11]#[N:12])=[N:6][C:7]([F:10])=[CH:8][N:9]=1

参与物

5

反应物 2

HCID 226627892-Pyrazinecarbonitrile, 3-azido-6-fluoro-HCID 178418361HCID 178418361，化合物2 次

产物 1

HCID 22662784HCID 22662784，化合物收率 38.6%

试剂、催化剂与溶剂 2

HCID 17803853Palladium on calcium carbonate催化剂HCID 887(5BETA,17BETA)-17-羟基-17-(甲基-D3)-2'H-雄甾-2-烯并[3,2-C]吡唑-5'(1'H)-酮溶剂

实验过程

In 5.0 mL of methanol was dissolved 0.24 g of 3-azido-6-fluoro-2-pyrazinecarbonitrile. After adding 0.075 g of lead-poisoned palladium-calcium carbonate at room temperature, hydrogen gas was introduced into the mixture at room temperature under a pressure of 1 atmosphere until the mixture became showing no further adsorption of hydrogen. After filtering off the insoluble matter from the reaction mixture, the filtrate was concentrated under reduced pressure. The residue thus obtained was purified by silica gel column chromatography [eluent: chloroform] to obtain 0.078 g of 3-amino-6-fluoro-2-pyrazinecarbonitrile as a yellow-colored solid product.

后处理

  1. filtrationAfter filtering off the insoluble matter from the reaction mixture
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. customThe residue thus obtained
  4. customwas purified by silica gel column chromatography [eluent: chloroform]

来源与证据

ORD记录
ord-4480d28c37a24f63a3f2cd8e179bbf7d
来源数据集
uspto-grants-2004_10
专利号
US06800629B2

关联笔记

加载中…