반응 #55509

반응 방정식

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

dimethylformamide

chloroformic acid 2-methoxyethyl ester

→

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

용매

triethylamine

반응 조건

후처리

1. 1
   온도The 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
   기타The precipitate obtained
5. 5
   여과is filtered off
6. 6
   세척washed with methylene chloride, methanol and water
7. 7
   세척The filtrate is washed with water
8. 8
   건조dried over sodium sulfate
9. 9
   농축By concentrating the solvent

실험 절차

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.

출처