Dimethylformamide → HCID 86630158, compound

Participants

Reaction Steps

28 mg of 2-(3,4-dichlorophenyl)-3-hydroxy-4-methylcarbonylthiophene (synthesized in accordance with WO2004/108683) and 29.7 mg of 5-(4-isopropylpiperazine-1-carbonyl)thiophene-2-carbohydrazide prepared in Reference Synthetic Example 1 in 2 mL of isopropyl alcohol were heated with 3 mg of p-tosylic acid monohydrate and 25 μL (1 eq) of 4 M hydrogen chloride/dioxane at 105° C. for 8 hours. The reaction solution was further heated with 2 mL of dimethylformamide at 105° C. for 5 hours and cooled to room temperature. The precipitated solid was recovered by filtration and washed with 1 mL of isopropyl alcohol and 1 mL of chloroform, and the resulting crystals were dried to give the desired product (yield 54%).

Provenance & Evidence