ChemicalBook CAS DataBase List 2,3-Dichloropyrazine

2,3-Dichloropyrazine synthesis

10synthesis methods

Product Name:2,3-Dichloropyrazine
CAS Number:4858-85-9
Molecular formula:C4H2Cl2N2
Molecular Weight:148.98

6863-76-9
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4858-85-9
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Yield:-

Reaction Conditions:

with trichlorophosphate at 60; for 1 h;Heating / reflux;

Steps:

46.2
3-CHLOROPYRAZINE 1-oxide (D46, Step 1) (2.2 g, 16.9 MMOL) was added slowly to phosphorus oxychloride (10 ml) at 60 °C. When the addition was complete the mixture was heated at reflux for 60 minutes. The mixture was allowed to cool and poured into ice and solid sodium acetate (5 g). This was stirred until the ice had melted and then extracted with DICHLOROMETHANE. The DICHLOROMETHANE extracts were combined, washed with saturated sodium bicarbonate solution, water and brine. The organic portion was dried under sodium sulfate and evaporated in vacuo. The resulting residue was purified by column chromatography ELUTING with a mixture of ethyl acetate: hexane (1: 20) to afford the title compound (0.86 g). 'H NMR (CDCI3) 8.32 (2H, s).

References:

GLAXO GROUP LIMITED WO2004/56369, 2004, A1 Location in patent:Page/Page column 23

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14508-49-7 Synthesis