Reference of 4774-14-5,Some common heterocyclic compound, 4774-14-5, name is 2,6-Dichloropyrazine, molecular formula is C4H2Cl2N2, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
Example 11 3, 5-DICHLORO-2-METHYLPYRAZINE To a solution of n-butyllithium (3.8 mL, 2.5M in hexane, 9.4 mmol) in THF (40mL) cooled to – 30 C under nitrogen was added 2,2, 6,6-tetramethylpiperidine (1.7 mL, 10.1 mmol). This solution was allowed to warm to 0 C over 20 min. and was then cooled TO-70C. A solution of 2,6-dichloropyrazine (1 g, 6.7 mmol) in THF (40 mL) was added dropwise and the resulting brown solution stirred at-70C for 30 min. LODOMETHANE (4.1 mL, 67 mmol) was then added and the solution stirred at-70C for a further 45 min after which time a mixture of ethanol (5 mL), THF (5 mL) and 1N HCl (1 mL) was added. The solution was allowed to warm to room temperature and was concentrated under reduced pressure. The residue was dissolved in H20 (50 mL) and the product extracted into dichloromethane (3 x 30 mL). The combined organic layers were washed with H2O (50 mL) and brine (50 mL) and dried (NA2SO4). The organic layer was concentrated in vacuo and the residue purified by column chromatography eluting with dichloromethane-hexane (1: 1) to separate the product as a clear motile oil (820 mg). ‘H-n. m. r. (CDC13) 82.65 (s, 3H, CH3), 8.41 (s, 1H, pyraz.-H).
The synthetic route of 4774-14-5 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; CYTOPIA PTY LTD; WO2004/52868; (2004); A1;,
Pyrazine – Wikipedia,
Pyrazine | C4H4N2 – PubChem