Triethylamine → HCID 86660115, compound

Participants

Reaction Steps

2-(4-(5-Bromopyrimidin-2-ylamino)phenoxy)ethanol 10 (26.6 mmol) is dissolved in DCM (50 mL) followed by addition of MsCl (32 mmol). The reaction vessel is chilled in an ice-water bath and triethylamine (53.3 mmol) is added slowly. The mixture is stirred at rt for 16 h. The solvent is removed and the residue is triturated with water (300 mL). The solid is filtered and dried under vacuum for 12 h to give 2-(4-(5-Bromopyrimidin-2-ylamino)phenoxy)ethyl methanesulfonate 11 as off-white solid. 1H NMR (400 MHz, d6-DMSO) δ 9.71 (s, 1H), 8.54 (s, 2H), 7.59 (d, J=9.2 Hz, 2H), 6.93 (d, J=9.2 Hz, 2H), 4.52 (m, 2H), 4.22 (m, 2H), 3.24 (s, 3H). MS (m/z) (M+1)+: 388.0, 340.0.

Provenance & Evidence