反应详情

温度

5 °C

In a 1 liter-four-necked flask, 93.7 (1.28 mol) of N,N-dimethylformamide was placed and cooled to 5° C., followed by addition of 107.4 g (7.00×10-1 mol) of POCl3 in 15 min. below 10° C. under stirring. After stirring for 30 min. below 10° C., 160 g (6.35×10-1 mol) of 2-dodecylthiophene was added dropwise to the mixture in 10 min. at room temperature, followed by stirring for 1.5 hours and further stirring for 2.5 hours at 60° C. After the reaction, the reaction mixture was poured into 2 liters of iced water, subjected to 3 times of extraction with 500 ml of chloroform and washed 6 times with 500 ml of water. The organic layer was dried on CaCl2, followed by distilling-off of the solvent to obtain 237 g of a crude product. The crude product was subjected to reduced-pressure distillation in an atmosphere of nitrogen to obtain 135 g of a product (yield: 75.9%). b.p.: 160° C./0.6 mmHg

1. stirringAfter stirring for 30 min. below 10° C.
2. stirringby stirring for 1.5 hours
3. stirringfurther stirring for 2.5 hours at 60° C
4. customAfter the reaction
5. extractionsubjected to 3 times of extraction with 500 ml of chloroform
6. washwashed 6 times with 500 ml of water
7. customThe organic layer was dried on CaCl2
8. customto obtain 237 g of a crude product
9. distillationThe crude product was subjected to reduced-pressure distillation in an atmosphere of nitrogen