Methanesulfonic Acid → HCID 86750597, compound

Participants

Reaction Steps

A mixture of 1-ethyl-6-methoxy-N-(4-methoxyphenylmethyl)-1H-pyrazolo[3,4-b]quinolin-4-amine (1.0 g, 2.76 mmol), boron tribromide (6 ml, 6 mmol) and 1,2-ethylenedichloride (30 ml) is stirred at room temperature overnight. The reaction mixture is poured into water and then is basified with NaOH. The layers are separated, and then the aqueous layer is acidified with acetic acid. The precipitate that forms is collected by filtration, washed with water and dried to afford the product as the free base. The free base is taken up in methanol and treated with methanesulfonic acid. The methanol is evaporated and the solid residue is recrystallized from 2-propanel/methanol/ether and dried in vacuo to afford 350 mg of 1-ethyl-6-hydroxy-N-(4-hydroxyphenyl methyl)-1H-pyrazolo[3,4-b]quinolin-4-amine.CH3SO3H.

Provenance & Evidence