2-Amino-5-chloropyridine → 2-Amino-5-chloro-3-iodopyridine

温度

55 °C

A mixture of 6.43 g of 5-chloropyridin-2-ylamine and 12.38 g of N-iodosuccinimide in 300 ml of glacial acetic acid is heated at around 55° C. for 6 hours. After returning to a temperature of approximately 20° C., the mixture is agitated for approximately 18 hours and then concentrated to dryness under reduced pressure (13 kPa). The residue is taken up with 400 ml of water; the pH of the suspension obtained is brought back to approximately 8 by adding a saturated aqueous sodium hydrogen carbonate solution. The precipitate is filter-dried, washed with water, and dried at 40° C. under reduced pressure (13 kPa) for approximately 3 hours. 12.35 g of 5-chloro-3-iodopyridin-2-ylamine are obtained in the form of a solid, the characteristics of which are as follows:

1. customAfter returning to a temperature of approximately 20° C.
2. concentrationconcentrated to dryness under reduced pressure (13 kPa)
3. customthe pH of the suspension obtained
4. customThe precipitate is filter-dried
5. washwashed with water
6. customdried at 40° C. under reduced pressure (13 kPa) for approximately 3 hours

ORDレコード

ord-506e8cb1709847888265fbbfa270d949

出典データセット

uspto-grants-2009_05

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07528147B2