反应详情

温度

80 °C

2-Bromobutyric acid, (200 g, 1.2 mol), sodium benzenesulfinate,(236 g, 1.44 mol) and water(1000 mL) were heated to 80° C. After about 1 hour the clear solution had turned cloudy and an oil had precipitated out. After heating at 80° C. for a total of 2 hours the mixture was cooled with good stirring. The oil solidifies and the crystals were filtered off, washed with water and air-dried. Yield 162.5 g. 2-Phenylsulfonylbutyric acid (47.8 g, 0.21 mol) was suspended/dissolved in ethyl acetate (400 mL) to which was added DMF (0.5 mL), thionyl chloride (76 mL, 1.05 mol) and the mixture heated to 70° C. for 2 hrs. After this period the solution was cooled, concentrated under reduced pressure and co-evaporated with ethyl acetate (×1). The resulting pale yellow oil was used as such in the preparation of inventive coupler IC-1.

1. customan oil had precipitated out
2. temperaturewas cooled with good stirring
3. filtrationthe crystals were filtered off
4. washwashed with water
5. customair-dried
6. temperaturethe mixture heated to 70° C. for 2 hrs
7. temperatureAfter this period the solution was cooled
8. concentrationconcentrated under reduced pressure and co-evaporated with ethyl acetate (×1)
9. customsuch in the preparation of inventive coupler IC-1