反応 #3277

反応方程式

m-chloroperbenzoic acid

6-(2,6-dichlorophenyl)-8-methyl-2-methylsulfanyl-8H-pyrido[2,3-d]pyrimidin-7-one

6-(2,6-Dichlorophenyl)-8-methyl-2-methylsulfanyl-8H-pyrido[2,3-d]pyrimidin-7-one

dimethylsulfoxide

→

6-(2,6-Dichlorophenyl)-2-methanesulfonyl-8-methyl-8H-pyrido[2,3-d]pyrimidin-7-one

溶媒

chloroform

反応条件

後処理

1. 1
   workup.WAITAfter 15 minutes
2. 2
   洗浄the chloroform solution was washed with 30 mL of saturated sodium bicarbonate
3. 3
   乾燥The separated organic layer was dried over sodium sulfate
4. 4
   ろ過filtered
5. 5
   濃縮concentrated to ca. 5 mL volume
6. 6
   その他Crystals separated
7. 7
   workup.ADDITIONAdded ca. 5 mL of petroleum ether
8. 8
   ろ過filtered

実験手順

A quantity of 0.346 g (1.00 mmol) of 50% to 60% m-chloroperbenzoic acid (assuming 50% peracid was present) was added at 25° C. to a stirred solution of 0.165 g (0.47 mmol) of 6-(2,6-dichlorophenyl)-8-methyl-2-methylsulfanyl-8H-pyrido[2,3-d]pyrimidin-7-one of Example 37 in 15 mL of chloroform, and the solution was stirred overnight. A quantity of 0.25 g (3.20 mmol) of dimethylsulfoxide was added to reduce any excess peracid. After 15 minutes, the chloroform solution was washed with 30 mL of saturated sodium bicarbonate and then with water. The separated organic layer was dried over sodium sulfate, filtered, and concentrated to ca. 5 mL volume. Crystals separated. Added ca. 5 mL of petroleum ether and filtered; wt 0.165 g (92%); mp >290° C.

出典