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ChemicalBook CAS DataBase List Raltitrexed

Raltitrexed synthesis

14synthesis methods
132463-02-6 Synthesis
Diethyl N-[5-[N-[(3,4-dihydro-2-methyl-4-oxo-6-quinazolinyl)methyl]-N-methylamino]-2-thenoyl]-L-glutamate

132463-02-6
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Yield:112887-68-0 80%

Reaction Conditions:

with sodium hydroxide in water at 25;

Steps:

9 Preparation of Compound 1

To the reaction flask, 1.35 g of sodium hydroxide and 3.3 ml of water were added, and the mixture was cooled to 25 °C or lower, and 1.35 g of the starting material (Compound 2) was slowly added with stirring. The mixture was further stirred for 1.5 to 2 hours, and then the reaction solution (2 × 27ml), water phase filtration. The filtrate was stirred with 2M hydrochloric acid to adjust the pH to 3.0, and the mixture was stirred for 2 hours. The product was washed with distilled water and the solid was dried under vacuum at 80 °C for 10 hours to give 0.96 g of product, 80% yield and 99.5% HPLC purity.

References:

CN106957296,2017,A Location in patent:Paragraph 0064; 0065

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