4,6-Dichloro-2-methylpyrimidine synthesis
- Product Name:4,6-Dichloro-2-methylpyrimidine
- CAS Number:1780-26-3
- Molecular formula:C5H4Cl2N2
- Molecular Weight:163
1194-22-5
1780-26-3
General procedure for the synthesis of 4,6-dichloro-2-methylpyrimidine from 6-hydroxy-2-methylpyrimidin-4-one: 4,6-dihydroxy-2-methylpyrimidine (5.0 g, 0.04 mol) was added to a mixed solution of thionyl chloride (18.9 g, 0.16 mol) with acetonitrile. The reaction mixture was stirred at 80 °C for 3 h and the completion of the reaction was monitored by thin layer chromatography (TLC). After completion of the reaction, excess thionyl chloride was removed by distillation under reduced pressure and the residue was slowly poured into 50 g of ice water. The precipitated solid was filtered and purified by column chromatography to give 6.1 g (yield: 94%) of 4,6-dichloro-2-methylpyrimidine as a white solid.
1194-22-5
135 suppliers
$6.00/5g
1780-26-3
478 suppliers
$10.00/10g
Yield:1780-26-3 94%
Reaction Conditions:
with thionyl chloride in acetonitrile at 80; for 3 h;Industrial scale;Temperature;Concentration;Reagent/catalyst;
Steps:
3.1 first step: Synthesis of 4,6-Dichloro-2-methylpyrimidine
4,6-dihydroxy-2-methylpyrimidine (5.0 g, 0.04 mol) was added to a mixed solution of thionyl chloride (18.9 g, 0.16 mol) and acetonitrile,The reaction was stirred at 80 ° C for 3 hours, and the plate was confirmed to disappear. The excess thiophenolate was distilled off under reduced pressure and the residue was poured into 50 g of ice water. The precipitated solid was filtered and purified by column chromatography to give 6.1 g (yield: 94%) of solid.
References:
Shanghai ZaiQi Bio-Tech Co., Ltd,;Wang, Zhiguo;Song, Yanhong;Ma, Xiujuan;Tian, Beibei;Li, Shijiang;Li, Chao;Li, Qiang;Li, Tao CN106478519, 2017, A Location in patent:Paragraph 0020-0023; 0030-0032; 0038-0040; 0049-0052
40497-30-1
339 suppliers
$14.00/5g
1780-26-3
478 suppliers
$10.00/10g