反应详情

Preparation analogous to 16), S43, using 16.1 g (100 mmol) of 2-tert-butyl-5-cyanopyrimidine [126230-72-6] and 71.4 g (300 mmol) of 3,4-diamino-6-tert-butylpyridine dihydrochloride (S50) instead of 25.9 g (100 mmol) of 2-N-pivaloylamido-3-cyano-6-tert-butylpyridine (S42) and 90.5 g (500 mmol) of o-phenylenediamine dihydrochloride [615-28-1]. After cooling, the violet melt is dissolved in a mixture of 150 ml of ethanol and 300 ml of water at elevated temperature, and a solution of 25 g of sodium carbonate in 100 ml of water is then added dropwise with vigorous stirring (note: foaming, evolution of carbon dioxide). When the addition is complete, the mixture is stirred for a further 30 min., the brown solid is then filtered off with suction, washed three times with 100 ml of water each time and dried in vacuo. Yield: 23.8 g (77 mmol), 77%. Purity: >95% according to 1H-NMR.

1. customPreparation analogous to 16), S43
2. temperatureAfter cooling
3. additionWhen the addition
4. filtrationthe brown solid is then filtered off with suction
5. washwashed three times with 100 ml of water each time
6. customdried in vacuo