ChemicalBook CAS DataBase List ethyl 4-((3-chloro-4-methoxybenzyl)amino)-2-hydroxypyrimidine-5-carboxylate

ethyl 4-((3-chloro-4-methoxybenzyl)amino)-2-hydroxypyrimidine-5-carboxylate synthesis

6synthesis methods

Product Name:ethyl 4-((3-chloro-4-methoxybenzyl)amino)-2-hydroxypyrimidine-5-carboxylate
CAS Number:330785-99-4
Molecular formula:C15H16ClN3O4
Molecular Weight:337.76

4-(3-chloro-4-MethoxybenzylaMino)-5-ethoxycarbonyl-2-MethylsulfinylpyriMidine

330785-82-5
59 suppliers
inquiry

ethyl 4-((3-chloro-4-methoxybenzyl)amino)-2-hydroxypyrimidine-5-carboxylate

330785-99-4
19 suppliers
inquiry

Yield:330785-99-4 65.06%

Reaction Conditions:

with water;sodium hydroxide in dichloromethane at -5 - 5; for 1.16667 h;

Steps:

1 Synthesis of the first intermediate

Compound 4-(3-Chloro-4-methoxybenzylamino)-5-ethoxycarbonyl-2-methylsulfinylpyrimidine (38.38 g,0.1 mol) into 150 mL of water and 100 mL of methylene chloride and start stirringAfter stirring for 10 minutes, the reaction vessel was placed in an ice bath and cooled to -5°C.Control temperature 0±5°C, slowly add (30g, 0.15mol) 20% aqueous sodium hydroxide solution,After completion of the dropwise addition, the reaction was incubated at -5 to 5°C for 1 hour, and the organic layer TLC (ethyl acetate:ethanol:ammonia water=4:1:0.1) was sampled.Until the compound 4-(3-chloro-4-methoxybenzylamino)-5-ethoxycarbonyl-2-methylsulfinylpyrimidine is not present, after the reaction is completed,Control the reaction system temperature ≤ 5 ° C drop 10% hydrochloric acid, adjust the system pH value is neutral,The organic layer was separated and the aqueous layer was extracted twice with dichloromethane and the organic layers were combined.Dry over anhydrous magnesium sulfate, filter, and distill off to obtain 21.95 g of a pale yellow solid.The purity was 99.9%; yield: 65.06%.

References:

CN107879986,2018,A Location in patent:Paragraph 0065; 0066

330785-82-5
59 suppliers
inquiry

330785-81-4 Synthesis