Hydrochloric Acid → 2-Iodo-4-methoxybenzoic acid

温度

75 °C

A mixture of 4-methoxyanthranilic acid (30.5 g, 0.18 mol), water (274.5 ml), and concentrated HCl (36.6 ml) was heated at 75° C. to effect solution and then was cooled to 0° C. The mixture was then treated with NaNO2 (13.3 g) in water (27.5 ml), followed by potassium iodide (45.75 g) in a water (75 ml)/H2SO4 (10.1 ml) solution. The reaction mixture was heated on a steam bath for 2 hours, then excess iodine was steam distilled. The reaction mixture was then cooled and the product was collected by filtration and dried in an oven at 75° C. To afford 39.28 g (78.6%) of crude product. The crude product was treated with toluene, the mixture was filtered and the filtrate was concentrated to afford 26.03 g of 2-iodo-4-methoxybenzoic acid.

1. temperaturewas cooled to 0° C
2. temperatureThe reaction mixture was heated on a steam bath for 2 hours
3. distillationdistilled
4. temperatureThe reaction mixture was then cooled
5. filtrationthe product was collected by filtration
6. customdried in an oven at 75° C
7. customTo afford 39.28 g (78.6%) of crude product
8. filtrationthe mixture was filtered
9. concentrationthe filtrate was concentrated

ORDレコード

ord-593e53600721465ca80007ad82b445f8

出典データセット

uspto-grants-1999_12

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US06008226