Benzene → 2-Dimethylaminopyridine

温度

70 °C

3.1 gm. of cobaltocene (0.016 mole) under nitrogen was dissolved in 44.0 gm. of benzol. The solution mixed with 164 gm. of anhydrous N,N-dimethylcyanamide (2.3 moles). The reaction mixture was saturated with 12 atm. of acetylene at 20° C. in a 1-liter autoclave (with stirring). The reaction mixture was heated to 70° C. Then at the beginning of the exothermal reaction, the heating was carefully increased so that a temperature of 160° C. prevailed in the autoclave. After a drop in pressure in the autoclave to below 12 atm., acetylene was repressed on. After 10 hours of reaction time, the autoclave was cooled down and expansion allowed. As a result of fractional distillation, 238 gm. of 2-(N,N-dimethylamino)-pyridine (boiling point: 92° C., 21 torr) was obtained, after benzol and a small quantity of N,N-dimethylcyanamide had been obtained. The 2-(N,N-dimethylamino)-pyridine had a purity of 99.8 percent--this corresponded to a yield of 84.5 percent.

1. additionThe solution mixed with 164 gm
2. customThen at the beginning of the exothermal reaction
3. temperaturethe heating was carefully increased so that a temperature of 160° C.
4. customAfter 10 hours of reaction time
5. temperaturethe autoclave was cooled down
6. customAs a result of fractional distillation, 238 gm

ORDレコード

ord-5d85a4687cd74782a6762d5c68f1f304

出典データセット

uspto-grants-1980_04

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US04196287