تفاعل #468844

ord-e7d529d8be244d7d90eb17fcd5e19dbd

معادلة التفاعل

Nc1nc(N)nc(N)n1
melamine
OCCOCCO
diethylene glycol
Nc1nc(N)nc(N)n1
melamine
[H][H]
hydrogen
OCCOCCNc1nc(NCCOCCO)nc(NCCOCCO)n1
2,4,6-tris(5-hydroxy-3-oxapentylamino)-1,3,5-triazine
Nc1nc(N)nc(NCCOCCO)n1
2,4-diamino-6-(5-hydroxy-3-oxapentylamino)-1,3,5-triazine
Nc1nc(NCCOCCO)nc(NCCOCCO)n1
2-amino-4,6-bis(5-hydroxy-3-oxapentylamino)-1,3,5-triazine

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITIONwas introduced under pressure at normal temperature
  2. 2
    أخرىreached 260° C.
  3. 3
    درجة الحرارةAfter cooling

الإجراء التجريبي

In a stainless steel autoclave of an inner volume of 100 ml, 1.26 g (10 mmol) of melamine, 250 mg of 5% Pd—C catalyst, 250 mg of manganese powder, and 30 ml of diethylene glycol were charged. After the inside of the reaction system was sufficiently substituted with nitrogen gas, 10 kg/cm2 of hydrogen gas was introduced under pressure at normal temperature. Then, the temperature was elevated while stirring, and after the temperature reached 260° C., the reaction was carried out at the same temperature for further 2 hours. After cooling, the reaction mixture was taken out and quantitative analysis of the reaction product was performed under the above analytical conditions. As a result, the reaction conversion rate of the starting material melamine was 64.3% and it was confirmed that there were produced 2,4-diamino-6-(5-hydroxy-3-oxapentylamino)-1,3,5-triazine in a yield of 25.8%, 2-amino-4,6-bis(5-hydroxy-3-oxapentylamino)-1,3,5-triazine in a yield of 20.0%, and 2,4,6-tris(5-hydroxy-3-oxapentylamino)-1,3,5-triazine in a yield of 6.5%, respectively.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06307046B1uspto-grants-2001_10