Hydrochloric Acid → HCID 11390207, compound

Participants

Reaction Conditions

Reaction Steps

Concentrated HCl (14 mL) was added to stirred ice cooled DMF (350 mL) followed by 7.14 g of 6-Hydrazino-5-nitroso-pyrimidine-2,4-diamine. After 5 min., chloroacetaldehyde diethylacetal (15.4 mL) was added over a ca. 2 min. period. The cooling bath was removed and the mixture allowed to come to room temperature. After 1 h, the mixture was warmed to 85° C. for 1.5 h and then allowed to cool to room temp over a 2.5 h period. The mixture was filtered to remove a small amount of brown insoluble material, the filtrate made alkaline with concentrated NH4OH solution and then diluted with an equal volume of water. The mixture was set aside for 1 h and then filtered to collect the orange/brown solid which was further dried in vacuo over P2O5 to give 3.50 g of 3-Chloromethyl-pyrimido[5,4-e][1,2,4]triazine-5,7-diamine 3.

Provenance & Evidence