2-Amino-3-chloropyrazine → HCID 86670917, 화합물

HRID 1186491노트

반응식

HRID 1186491 반응식
[Br:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH:8](Br)[CH:9](OC)OC)[N:3]=1.[Cl:15][C:16]1[C:17]([NH2:22])=[N:18][CH:19]=[CH:20][N:21]=1.CC1C=CC(S(O)(=O)=O)=CC=1.O>CC#N.O>[Br:1][C:2]1[N:3]=[C:4]([C:8]2[N:18]3[CH:19]=[CH:20][N:21]=[C:16]([Cl:15])[C:17]3=[N:22][CH:9]=2)[CH:5]=[CH:6][CH:7]=1

참가 물질

6

반응물 3

HCID 2762242-Amino-3-chloropyrazineHCID 521998p-Toluenesulfonic acid monohydrateHCID 866709182-Bromo-6-(1-bromo-2,2-dimethoxy-ethyl)-pyridine

생성물 1

HCID 86670917HCID 86670917, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 6342Acetonitrile용매

실험 절차

A mixture of 2-bromo-6-(1-bromo-2,2-dimethoxy-ethyl)-pyridine (from Example 37 supra) (5.267 g, 16.2 mmol), 3-chloropyrazin-2-amine (2.1 g, 16.2 mmol), and pTsOH.H2O (2.1 g, 11 mmol) in CH3CN (900 mL) and water (90 mL) was stirred and heated at reflux overnight. The reaction mixture was then cooled to room temperature, concentrated under reduced pressure. The crude product was purified by chromatography (CH2Cl2:CH3OH, 100:1) to give 3-(6-bromo-pyridin-2-yl)-8-chloro-imidazo[1,2-a]pyrazine. (Yield 4.86 g, 52%). LC-MS: [M+H]+ 309.

후처리

  1. temperatureheated
  2. temperatureat reflux overnight
  3. concentrationconcentrated under reduced pressure
  4. customThe crude product was purified by chromatography (CH2Cl2:CH3OH, 100:1)

출처 및 근거

ORD 기록
ord-3de223f2cfda423bb3228e612169f1f8
출처 데이터셋
uspto-grants-2014_03
특허 번호
US08673905B2

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