Sulfuric Acid → (2-Chloro-6-iodophenyl)acetic acid

Temperatur

115 °C

A mixture of 2-(2-chloro-6-iodophenyl)acetonitrile (10 g, 36 mmol) in 20 mL dioxane was treated with 25 mL 9M H2SO4. The mixture was stirred at 115° C. for 2 hours. The mixture was transferred into a sealed tube and heated to 150° C. and stirred for 2 hours. The mixture was then cooled to room temperature and diluted with 100 mL water. The mixture was extracted with EtOAc (3×50 mL). The combined organic layers were washed with saturated NaCl (20 mL), dried over sodium sulfate, and concentrated to give crude product 10.3 g as pale yellow solid. MS m/e: (M+H)+ 297.

1. customThe mixture was transferred into a sealed tube
2. temperatureheated to 150° C.
3. stirringstirred for 2 hours
4. temperatureThe mixture was then cooled to room temperature
5. extractionThe mixture was extracted with EtOAc (3×50 mL)
6. washThe combined organic layers were washed with saturated NaCl (20 mL)
7. dry with materialdried over sodium sulfate
8. concentrationconcentrated

ORD-Eintrag

ord-3ae46ba2925a438d8a3994de3bdc0e2a

Quelldatensatz

uspto-grants-2011_04

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07928139B2