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ChemicalBook CAS DataBase List 5-Chloroimidazo[1,2-a]pyrazine
63744-41-2

5-Chloroimidazo[1,2-a]pyrazine synthesis

2synthesis methods
-

Yield:63744-41-2 73%

Reaction Conditions:

in 1,2-dimethoxyethane;water at 60; for 1.5 h;

Steps:

59

To a solution of 6-chloropyrazin-2-amine (0.5 g, 3.86 mmol) in DME (3 mL) at room temperature was slowly added 2-chloroacetaldehyde (45% aqueous solution, 2.4 mL, 14 mmol). The resulting mixture was heated to 66 °C for 90 minutes, cooled to room temperature, and then basified with IN NaOH. This basified mixture was extracted with EtOAc (2x). The combined organic layers were washed with brine, dried over sodium sulfate and concentrated. The crude material was purified by silica gel chromatography (eluting with 0-10% MeOH in DCM) to provide Intermediate 59 (430 mg, 73% yield). MS (ES): m/z= 153.9 [M+H]+. XH NMR (400 MHz, DMSO-d6) δ ppm 9.12 (1 H, s), 8.27 (1 H, s), 8.15 (1 H, s), 7.85 (1 H, s). Intermediate 59 was used in the synthesis of Example 251.

References:

WO2012/15723,2012,A1 Location in patent:Page/Page column 106; 107

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