MEPANIPYRIM synthesis
- Product Name:MEPANIPYRIM
- CAS Number:110235-47-7
- Molecular formula:C14H13N3
- Molecular Weight:223.27
Yield:110235-47-7 90%
Reaction Conditions:
with bis-triphenylphosphine-palladium(II) chloride;copper(l) iodide;triethylamine in 1,4-dioxane at 100; for 12 h;Inert atmosphere;
Steps:
1.4 (4) Synthesis of Mepanipyrim
Ar atmosphere, at room temperature into PdCl2 (PPh3)2 (0·01mmol, 10 mg, 0.1mol %), CuI (0.5mmol, 5mol %) and 2-chloropyrimidinamine (10·0mmol) Anhydrous anaerobic dioxide (30mL) solution added the 10mL of Et3N, pass through the propyne gas, warm up at 100 ° C, stir the reaction for 12 h, cool at the greenhouse, the reaction is quenched by the addition of saturated NH4C1 (10mL), extracted with ethyl acetate three times, the organic phase is washed with a saturated NaCl solution, NaS04 drying, the solvent is distilled off under reduced pressure, the crude product was re-crystallized from n-hexane/isopropyl ether (ν/ν = 1/1), obtained product (2.0 g, yield 90%). The total yield of Mepanipyrim is 45%.
References:
Northwest Normal University;Quan Zhengjun;Yan Zhongfei;Wang Xicun CN104003944, 2016, B Location in patent:Paragraph 0014; 0018
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