反应详情

温度

50 °C

In a 5 liter-five-necked flask, 266 g (1.0 mol) of 2-dodecanoylthiophene, 392.4 ml of 60% hydrazine hydrate and 3 liter of diethyleneglycol were placed and reacted for 6 hours at 195° C. with distilling-off of excessive water and hydrazine hydrate. The mixture was cooled to 50° C. and 210.6 g of KOH was added thereto, followed by heating again to react for 2.5 hours at 155° C. After the reaction, the reaction mixture was poured into 10 liter of water, extracted two times with 2 liter of isopropyl ether, followed by drying with CaCl2 and distilling-off of the solvent to obtain 229 g of a crude product. The crude product was subjected to reduced-pressure distillation in an atmosphere of nitrogen to obtain 168 g of a pure product (yield: 66.7%). b.p.: 121.5° C./0.7 mmHg

1. temperatureby heating again
2. customto react for 2.5 hours at 155° C
3. customAfter the reaction
4. extractionextracted two times with 2 liter of isopropyl ether
5. dry with materialby drying with CaCl2 and distilling-off of the solvent
6. customto obtain 229 g of a crude product
7. distillationThe crude product was subjected to reduced-pressure distillation in an atmosphere of nitrogen