反应详情

温度

-60 °C

To a solution of 1.5 g of 3-(5-fluorobenzothiazol-2-yl-trans-ethenyl)benzyl alcohol (Preparation H2) in 40 ml of methylene chloride and 25 ml of dimethylsulfoxide at -60° C. was added a solution of 0.64 ml of oxalyl chloride in 20 ml of dry methylene chloride containing 0.74 ml of dimethylsulfoxide. After stirring at -60° C. for 35 minutes the reaction mixture was allowed to warm to -35° C. for 25 minutes. The mixture was again cooled to -60° C. and 3.65 ml of triethylamine was added over a period of 5 minutes. The mixture was allowed to warm to room temperature and was treated with 200 ml of water. The organic phase was washed with a brine solution, dried over sodium sulfate and concentrated in vacuo to give after trituration with ethyl acetate--hexane 1.2 g. A sample was recrystallized from ethyl acetate--hexane, m.p. 151°-152° C.

1. temperatureto warm to -35° C. for 25 minutes
2. temperatureThe mixture was again cooled to -60° C.
3. temperatureto warm to room temperature
4. washThe organic phase was washed with a brine solution
5. dry with materialdried over sodium sulfate
6. concentrationconcentrated in vacuo
7. customto give after trituration with ethyl acetate
8. customA sample was recrystallized from ethyl acetate