Hydrochloric Acid → HCID 54389688, compound

Participants

Reaction Steps

15 g 4-(4-chlorobenzyl)-2-(5-methylamino-1-carboxymethyl-3-pentyl)1(2H)-phthalazinone (Example 2) are dissolved in 150 ml methanol and reacted with 21 ml 5M sodium hydroxide solution. The solution is heated for 1.5 hours to 50° C., then concentrated in a rotary evaporator, and the residue reacted is with 105 ml 1M HCl (pH 6). The aqueous solution is first shaken with diethylether to remove nonpolar impurities and then extracted with dichloromethane. The combined dichloromethane phases are concentrated, and the raw product is crystallized from ethanol. The crystalline product is precipitated absorptively with ether and dried in a vacuum (55° C./2 Torr).

Provenance & Evidence