反应详情

温度

110 °C

To a solution of 2,6-dichloro-3-methoxyphenylisocyanate (preparation 1, 52.3 mg, 0.24 mmol, 1.2 eq.) in toluene (2.5 ml) is added N-methyl-N′-[4-(4-methyl-piperazin-1-yl)-phenyl]-pyrimidine-4,6-diamine (59.7 mg, 0.2 mmol, 1.0 eq.). The obtained suspension is stirred under argon at 110° C. for 17 h. After cooling the crude product is filtered off und purified by flash chromatography (100% DCM to 5% MeOH in DCM within 35 min). Fractions containing the product are pooled and evaporated to dryness. The residue is triturated with ether (2 ml) and treated with ultra sound until a homogeneous suspension is obtained. The precipitate is filtered off and vacuum dried at 60° C. over night to afford the title compound as a colorless powder: m.p. 161.5-163° C., HPLC: tR=5.07 min (purity: >99%, gradient A), ESI-MS: 516.6/518.5/520.4 [MH]+.

1. filtrationis filtered off
2. customund purified by flash chromatography (100% DCM to 5% MeOH in DCM within 35 min)
3. additionFractions containing the product
4. customevaporated to dryness
5. customThe residue is triturated with ether (2 ml)
6. additiontreated with ultra sound until a homogeneous suspension
7. customis obtained
8. filtrationThe precipitate is filtered off
9. customvacuum dried at 60° C. over night