ethyl 4-((3-chloro-4-methoxybenzyl)amino)-2-hydroxypyrimidine-5-carboxylate synthesis
- 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
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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
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![5-Pyrimidinecarboxylic acid, 4-[[(3-chloro-4-methoxyphenyl)methyl]amino]-2-(2-pyridinylmethoxy)-, 2-pyridinylmethyl ester](/CAS/20210305/GIF/372117-77-6.gif)
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330785-81-4
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$14.00/1g
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