Cesium carbonate → 2-Chloro-5-methyl-N-(2,3-dimethylphenyl)pyrimidin-4-amine

A mixture of 2-chloro-5-methylpyrimidin-4-amine (143.6 mg, 1 mmol), 1-bromo-2,3-dimethylbenzene (222 mg, 1.2 mmol), Pd2(dba)3 (92 mg, 0.1 mmol), Xantphos (174 mg, 0.3 mmol) and cesium carbonate (1.3 g, 4 mmol) were suspended in dioxane (150 mL) and heated at reflux under the argon atmosphere for 20 h. The mixture was filtered and the filtrate concentrated in vacuo. The residue was dissolved in EtOAc (10 mL) and added hexanes (100 mL). The solid was collected by filtration and washed with hexanes to afford the crude title compound as a yellow solid.

1. temperatureheated
2. temperatureat reflux under the argon atmosphere for 20 h
3. filtrationThe mixture was filtered
4. concentrationthe filtrate concentrated in vacuo
5. dissolutionThe residue was dissolved in EtOAc (10 mL)
6. additionadded hexanes (100 mL)
7. filtrationThe solid was collected by filtration
8. washwashed with hexanes

ORD-Eintrag

ord-95e1ea27c6ca46138a74577cde58013f

Quelldatensatz

uspto-grants-2012_03

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08133900B2