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ChemicalBook CAS DataBase List 2-[(6-Chloro-4-pyriMidinyl)oxy]-α-(diMethoxyMethyl)benzeneacetic Acid Methyl Ester
143230-42-6

2-[(6-Chloro-4-pyriMidinyl)oxy]-α-(diMethoxyMethyl)benzeneacetic Acid Methyl Ester synthesis

11synthesis methods
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Yield:143230-42-6 85%

Reaction Conditions:

Stage #1: 3-(α-methoxy)methylene benzofuran-2-(3H)-ketone;sodium methylatewith 2-methyl-1,4-divinylpiperazine in methanol;acetonitrile at 15 - 20; for 0.5 h;
Stage #2: 4,6-dichloropyrimidine in methanol;acetonitrile; for 1 h;Solvent;Temperature;

Steps:

4

A 500 ml three-necked flask was charged with 46.6 g of compound A (98%, 0.26 mol), 130 ml of acetonitrile, stirred at room temperature, and then put 0.4 g of 2-methyl-divinylpiperazine, , the mixture was stirred,cooled to 15 ° C and 53.8 g of sodium methoxide of methanol (28.87%, 0.287 mol) was added dropwise. The dropwise addition was controlled for half an hour. After the addition was completed, the mixture was incubated at 20 ° C for 1 hour. Then add 46.6 g of dichloropyrimidine(98.5%, 0.308mol) .After 1h it was acidified by adding 36% hydrochloric acid to pH = 4, washed twice with water and agitated, and the crude compound B was obtained by desolvation. The yield was 85%.

References:

CN104725321,2017,B Location in patent:Paragraph 0020; 0021; 0025; 0027