Sodium Hydroxide → 2,3-Dichloro-5-hydroxypyridine

温度

0 °C

At 0° C., a solution of 13 g of sodium hydroxide in 80 ml of water was added to 16 g of 5-acetyloxy-2,3-dichloropyridine in 100 ml of ice-water. The mixture was subsequently initially stirred at 0° C. for one hour and then at approximately 20° C. for 17 hours, and the reaction mixture was then washed with 150 ml of ethyl acetate. The mixture was acidified up to a pH of 4-5 by addition of acetic acid and then extracted three times with 100 ml of ethyl acetate each time. The combined organic phases were dried over magnesium sulfate and finally concentrated. Yield: 12.2 g.

1. waitat approximately 20° C. for 17 hours
2. washthe reaction mixture was then washed with 150 ml of ethyl acetate
3. additionThe mixture was acidified up to a pH of 4-5 by addition of acetic acid
4. extractionextracted three times with 100 ml of ethyl acetate each time
5. dry with materialThe combined organic phases were dried over magnesium sulfate
6. concentrationfinally concentrated

ORDレコード

ord-74aee886a2c74b9d862e2dd853fd9b8f

出典データセット

uspto-grants-2002_08

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US06432880B1