反应详情

温度

135 °C

To a stirred solution of Ethyl cyanoacetate (46.8 g, 414 mMol) and Triethyl orthoacetate (84.4 g, 520 mMol), in a 250 mL round bottom flask fitted with a short path distillation head, was added HOAc (1.2 mL, 21 mMol). The reaction was slowly heated to 135° C. and maintained at that temperature to distill off the ethyl alcohol that was produced. (Distillation started at ˜106° C.) At 15 min. intervals HOAc (1.2 mL, 21 mMol) was added to the reaction for an additional three times. The reaction was then slowly heated to 150° C. then cooled back down to ˜80° C. The title product (62.64 g, 82%) was obtained by short path distillation under high vacuum (bp 128° C., HV) as a pale yellow crystalline solid. (Note; Cooling to the condenser was shut off to prevent plugging.): 1H NMR (400 MHz, CDCl3) δ 4.27 (q, 2H), 4.22 (q, 2H), 2.61 (s, 3H), 1.43 (t, 3H), 1.31 (t, 3H).

1. temperaturemaintained at that temperature
2. distillationto distill off the ethyl alcohol that
3. customwas produced
4. additionwas added to the reaction for an additional three times
5. temperatureThe reaction was then slowly heated to 150° C.
6. temperaturethen cooled back down to ˜80° C