反应详情

A solution of 70 mg of 5-methyl-pyridine-2-sulfonic acid [2-(2-aminomethyl-pyridin-4-yl)-6-methoxy-5-(2-methoxy-phenoxy)-pyrimidin-4-yl]-amide hydrochloride, product of example 30 b), in toluene (5 ml), was treated at RT with 26 mg of triethyamine then with 10 mg of ethylisocyanate and refluxed for 1 h until the reaction was complete according to TLC analysis (CH2Cl2/MeOH: 95/5). The mixture was poured into cold diluted HCl and the product extracted into CH2Cl2. The organic layer was dried over Na2SO4 and the solvent removed in vacuo. The solid residue was crystallised from CH2Cl2/Et2O to afford 5-methyl-pyridine-2-sulfonic acid [2-{2-[(3-ethyl-ureido)-methyl]-pyridin-4-yl}-6-methoxy-5-(2-methoxy-phenoxy)-pyrimidin-4-yl]-amide as off-white crystals. ISP mass spectrum, m/e 580.1 (M+1 calculated for C27H29N7O6S: 580).

1. extractionthe product extracted into CH2Cl2
2. dry with materialThe organic layer was dried over Na2SO4
3. customthe solvent removed in vacuo
4. customThe solid residue was crystallised from CH2Cl2/Et2O