反应详情

A mixed solution comprising 1.49 g of methanesulfonyl chloride and 10 ml of acetonitrile was cooled with ice, and 10 ml of an acetonitrile solution comprising 1.3 g of monomethyl maleate and 1.34 g of pyridine was dropwise added thereto under cooling with ice over a period of 5 minutes, followed by stirring for 5 minutes at the same temperature. 10 ml of an acetonitrile solution comprising 1.72 g of 5-chloroanthranilic acid and 2.77 g of pyridine was added under cooling with ice over a period of 2 minutes, followed by rinsing with 5 ml of acetonitrile and stirring for 20 minutes at the same temperature. 1.49 g of methanesulfonyl chloride was added over a period of 2 minutes under cooling with ice, followed by rinsing with 2 ml of acetonitrile and stirring for 30 minutes, and then the temperature was returned to room temperature, followed by reaction for 4 hours. The reaction liquid was poured to 20 ml of water, followed by stirring for 30 minutes. The resulting crystals were collected by filtration, washed with water and a mixed liquid of acetonitrile:water (2:1), and dried to obtain 1.82 g of the brown desired product (melting point: 162 to 164° C.).

1. additionwas dropwise added
2. temperatureunder cooling with ice over a period of 5 minutes
3. additionwas added
4. temperatureunder cooling with ice over a period of 2 minutes
5. washby rinsing with 5 ml of acetonitrile
6. stirringstirring for 20 minutes at the same temperature
7. addition1.49 g of methanesulfonyl chloride was added over a period of 2 minutes
8. temperatureunder cooling with ice
9. washby rinsing with 2 ml of acetonitrile
10. stirringstirring for 30 minutes
11. customwas returned to room temperature
12. customfollowed by reaction for 4 hours
13. customThe reaction liquid
14. stirringby stirring for 30 minutes
15. filtrationThe resulting crystals were collected by filtration
16. washwashed with water
17. dry with materiala mixed liquid of acetonitrile:water (2:1), and dried