反应详情

温度

0 °C

(R)-4-(6-Benzyl-4,5-dimethyl-pyridazin-3-yl)-2-methyl-3,4,5,6-tetrahydro-2H-[1,2′]bipyrazinyl-5′-carboxylic acid (50 mg, 0.120 mmol) is dissolved in CH2Cl2 (300 μL). The mixture is cooled to 0° C. and oxalyl chloride (32 μL, 0.358 mmol) is added followed by DMF (3 drops). While stirring, the reaction is warmed to room temperature over 3 h. Diisopropylethylamine (209 μL, 1.2 mmol) is added dropwise followed by addition of N,O-dimethylhydroxylamine hydrochloride (14 mg, 0.144 mmol). Allow the reaction to stir for 16 h. Concentrate the crude mixture in vacuo. The residue is purified by flash chromatography on silica gel (MeOH/CH2Cl2) to afford the title compound (42 mg, 76%).

1. temperaturethe reaction is warmed to room temperature over 3 h
2. customthe reaction
3. stirringto stir for 16 h
4. concentrationConcentrate the crude mixture in vacuo
5. customThe residue is purified by flash chromatography on silica gel (MeOH/CH2Cl2)