2-Pyrazinecarbonitrile, 3-azido-6-fluoro- → HCID 22662784, 화합물

HRID 392347

반응식

HRID 392347 반응식
[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

참가 물질

5

반응물 2

HCID 226627892-Pyrazinecarbonitrile, 3-azido-6-fluoro-HCID 178418361HCID 178418361, 화합물2회

생성물 1

HCID 22662784HCID 22662784, 화합물수율 38.6%

시약·촉매·용매 2

HCID 17803853Palladium on calcium carbonate촉매HCID 887Methanol용매

실험 절차

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.

후처리

  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]

출처 및 근거

ORD 기록
ord-4480d28c37a24f63a3f2cd8e179bbf7d
출처 데이터셋
uspto-grants-2004_10
특허 번호
US06800629B2

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