反应 #956423

反应方程式

sodium hydroxide

water

5-chloro-6-ethyl-3-{[4-(methylsulfanyl)phenyl]amino}pyrazine-2-carboxamide

acetic acid

hydrogen peroxide

→

5-chloro-6-ethyl-3-{[4-(methylsulfonyl)phenyl]amino}pyrazine-2-carboxamide

溶剂

ethyl acetate

反应条件

后处理

1. 1
   workup.ADDITIONwere added
2. 2
   workup.ADDITIONwas added
3. 3
   workup.STIRRINGstirred for 30 minutes
4. 4
   其他the reaction liquid
5. 5
   其他was partitioned
6. 6
   干燥After drying over anhydrous sodium sulfate
7. 7
   过滤the organic layer was filtered
8. 8
   浓缩concentrated
9. 9
   洗涤The resulting residue was washed with ethyl acetate

实验过程

To a mixture of 5-chloro-6-ethyl-3-{[4-(methylsulfanyl)phenyl]amino}pyrazine-2-carboxamide (Preparation Example 394) (92 mg) and acetic acid (2.5 mL), sodium tungstate dihydrate (29 mg) and 30% hydrogen peroxide solution (0.15 mL) were added and stirred at room temperature for 30 minutes. After water and ethyl acetate were added to the reaction liquid, 1M aqueous sodium hydroxide was added and stirred for 30 minutes, and the reaction liquid was partitioned. After drying over anhydrous sodium sulfate, the organic layer was filtered and concentrated. The resulting residue was washed with ethyl acetate to give 5-chloro-6-ethyl-3-{[4-(methylsulfonyl)phenyl]amino}pyrazine-2-carboxamide (103 mg).

来源