Sodium Hydroxide → HCID 59020395, compound

Participants

Reaction Steps

A solution of 1.71 g (3.98 mmol) of 1-[3-(5-bromo-2-chloro-pyrimidin-4-ylamino)-propyl]-3-(3-nitro-phenyl)-urea in 50 ml of THF is mixed at room temperature with 30 ml of a 15% solution of Ti(III)Cl in approximately 10% hydrochloric acid. After 24 hours, another 5 ml of the 15% solution of Ti(III)Cl in approximately 10% hydrochloric acid is added. After another 6 hours, the batch is made basic with 2N NaOH solution and extracted from ethyl acetate. The combined organic phases are filtered through a Whatman filter and concentrated by evaporation. The residue that is obtained is purified by chromatography (DCM/EtOH 9:1). 850 mg (2.13 mmol, corresponding to 54% of theory) of the product is obtained.

Provenance & Evidence