تفاعل #55509

معادلة التفاعل

2,4-diamino-6-chloropyrimidine-3-oxide

dimethylformamide

chloroformic acid 2-methoxyethyl ester

→

2-methoxyethyl 2-amino-6-chloro-4-pyrimidinecarbamate-3-oxide

المذيبات

triethylamine

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةThe mixture is cooled for 2 hours
2. 2
   workup.STIRRINGstirred at room temperature for 16 hours
3. 3
   workup.DISTILLATIONThe solvent is distilled off at 25° C. in a high vacuum
4. 4
   أخرىThe precipitate obtained
5. 5
   ترشيحis filtered off
6. 6
   غسيلwashed with methylene chloride, methanol and water
7. 7
   غسيلThe filtrate is washed with water
8. 8
   تجفيفdried over sodium sulfate
9. 9
   تركيزBy concentrating the solvent

الإجراء التجريبي

5 G. of 2,4-diamino-6-chloropyrimidine-3-oxide are suspended in 50 ml. of dimethylformamide and 5 ml. of triethylamine and cooled to 0° C. while stirring. 4.3 G. of chloroformic acid 2-methoxyethyl ester are added dropwise to the cold suspension in the course of 15 minutes. The mixture is cooled for 2 hours and then stirred at room temperature for 16 hours. The solvent is distilled off at 25° C. in a high vacuum and the residue is digested with methylene chloride. The precipitate obtained is filtered off and washed with methylene chloride, methanol and water. The filtrate is washed with water and dried over sodium sulfate. By concentrating the solvent, there is obtained pure 2-methoxyethyl 2-amino-6-chloro-4-pyrimidinecarbamate-3-oxide having a melting point of 176°-178° C. Additional material is obtained by subjecting the mother liquor to chromatographical separation on silica gel.

المصدر