反应详情

温度

-10 °C

7-Mercapto-5-methyl-s-triazolo[1,5-a]pyrimidine-2-carboxylic acid dimethylacetamide (0.99 g) (3.33 mmol) is suspended in 15 ml of absolute dimethylacetamide and treated while stirring with 530 mg (3.96 mmol) of 1-chloro-N,N,2-trimethyl-1-propenamine. After 4 hours the solution is cooled to -10° C. and treated while stirring with 550 mg (6.6 mmol) of N-methylhydroxylamine hydrochloride and 860 mg (6.6 mmol) of ethyl-diisopropylamine. The reaction mixture is stirred at room temperature for 18 hours and subsequently concentrated in a high vacuum. The residue is crystallized using water and recrystallized from dimethylformamide/diethyl ether. There is obtained 0.50 g of N-hydroxy-7-mercapto-N,5-dimethyl-s-triazolo[1,5-a]pyrimidine-2-carboxamide as yellow crystals of melting point 215° C. (dec.).

1. additiontreated
2. additiontreated
3. concentrationsubsequently concentrated in a high vacuum
4. customThe residue is crystallized
5. customrecrystallized from dimethylformamide/diethyl ether