反应详情

At RT 60 mg (0.2 mmol) of 2-amino-6-[(2-aminoethyl)sulfanyl]-4-(4-hydroxyphenyl)-3,5-pyridinedicarbonitrile and 30 mg (0.3 mmol) of N-acetylimidazole are stirred in 0.5 ml of DMF for 1 hour. Water is slowly added dropwise, the mixture becomes slightly turbid and the crude product crystallizes out. The product is filtered off with suction, washed with water and dried under reduced pressure. This gives 53 mg of yellow crystals. The crystals are dissolved in 1 ml of a 1:1 mixture of CH2Cl2/CH3OH, and a few drops of concentrated ammonia are added (removal of diacetylated byproduct). The mixture is stirred at RT for 5 hours. The product crystallizes out when the reaction solution is concentrated. The product is filtered off with suction and washed with methanol.

1. customthe crude product crystallizes out
2. filtrationThe product is filtered off with suction
3. washwashed with water
4. customdried under reduced pressure
5. dissolutionThe crystals are dissolved in 1 ml of a 1:1 mixture of CH2Cl2/CH3OH, and a few drops of concentrated ammonia
6. additionare added
7. custom(removal of diacetylated byproduct)
8. customThe product crystallizes out when the reaction solution
9. concentrationis concentrated
10. filtrationThe product is filtered off with suction
11. washwashed with methanol