반응 #565311

반응 방정식

2-Bromobutyric acid

water

thionyl chloride

2-Phenylsulfonylbutyric acid

→

2-Phenylsulfonylbutyryl chloride

용매

DMF

ethyl acetate

반응 조건

후처리

1. 1
   기타an oil had precipitated out
2. 2
   온도was cooled with good stirring
3. 3
   여과the crystals were filtered off
4. 4
   세척washed with water
5. 5
   기타air-dried
6. 6
   온도the mixture heated to 70° C. for 2 hrs
7. 7
   온도After this period the solution was cooled
8. 8
   농축concentrated under reduced pressure and co-evaporated with ethyl acetate (×1)
9. 9
   기타such in the preparation of inventive coupler IC-1

실험 절차

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.

출처