تفاعل #2372707
ord-783c144d9c274407ac4058c3e392d279
معادلة التفاعل
المتفاعلات
الكواشف
المذيبات
ظروف التفاعل
المعالجة
- 1workup.STIRRINGhad first been stirred at room temperature for 5 hours
- 2workup.STIRRINGthe reaction mixture was subsequently stirred at 0°-5° C. for 24 hours
- 3درجة الحرارةwhile still cooling
- 4أخرىwas formed
- 5workup.DISTILLATIONThe methanol was distilled out of the reaction mixture in vacuo
- 6درجة الحرارةthe aqueous solution which remained was cooled
- 7أخرىthe product which had precipitated
- 8ترشيحwas then filtered off
الإجراء التجريبي
151.2 g (2 mols) of chloroacetonitrile were added to a solution of 10.8 g (0.2 mol) of sodium methylate in 500 ml of methanol at 0°-5° C., 117.6 g (2.2 mols) of ammonium chloride were then added at 15°-20° C. and the mixture was subsequently stirred at room temperature for 4 hours. Thereafter, it was added, at 0°-5° C., to a mixture of 208 g (2 mols) of methoxyacetic acid methyl ester, 120 g (2 mols) of formic acid methyl ester and 108 g (2 mols) of solid sodium methylate, which had first been stirred at room temperature for 5 hours. A solution of 108 g (2 mols) of sodium methylate in 400 ml of methanol was then added at 0°-5° C. and the reaction mixture was subsequently stirred at 0°-5° C. for 24 hours. The pH value was adjusted to 5 by adding concentrated hydrochloric acid, while still cooling, and water was then added in an amount such that a clear solution was formed. The methanol was distilled out of the reaction mixture in vacuo, the aqueous solution which remained was cooled, and the product which had precipitated was then filtered off. 140 g (40% of theory) of 2-chloromethyl-6-hydroxy-5-methoxypyrimidine were obtained in this manner in the form of a sand-colored powder with a melting point of 188° C. (decomposition). ##STR12##