* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
With sodium methylate; In 1,4-dioxane; diethyl ether; ethanol; hexane; water;
REFERENCE EXAMPLE 3 Preparation of 3-(4-bromo-2-fluorobenzyl)-5-methylthieno[2,3-d]-pyrimidine-2,4(1H,3H)-dione (Compound III-17) A solution of 3.71 g of ethyl 2-amino-4-methyl-3-thiophenecarboxylate and 7.91 g of trichloromethyl chloroformate in 50 ml of dioxane was stirred at a bath temperature of 80° to 100° C. for 3 hours, and the solvent was evaporated off under reduced pressure. The residue was dissolved in 30 ml of diethyl ether and 4.49 g of <strong>[112734-22-2]4-bromo-2-fluorobenzylamine</strong> was added dropwise thereto with ice-cooling. After the temperature of the mixture was raised to room temperature, the mixture was stirred for three hours, 20 ml of n-hexane was added dropwise thereto and a colorless precipitate was collected, giving 5.4 g of the ureide compound of the following formula in a yield of 68percent. STR10 A 5.3 g quantity of the ureide compound was dissolved in 70 ml of ethanol and 1.58 g of sodium methoxide was added thereto. The mixture was refluxed for 5 hours, concentrated to a half of volume, and then homogeneously mixed with 20 ml of water. The resulting solution was neutralized and acidified with concentrated hydrochloric acid to precipitate colorless crystals. The crystals were collected by filtration, washed with water and dried in vacuo, giving 4.75 g of the compound III-17 having a melting point of 296° to 297.5° C. in a yield of 97percent.
Chemistry
Pharmaceutical Intermediates
Inhibitors/Agonists
Material Science
For Research Only
120K+ Compounds
Competitive Price
1-2 Day Shipping
