HRID1632270

反应详情

EQUATION

反应方程式

HRID 1632270 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of phenyllithium in 150 milliliters 7:3 benzene-ether (0.1 mole) at 0° C. was slowly added a solution of 13.6 grams of tetramethylpyrazine (0.1 mole). The mixture was stirred at room temperature for 2 hours and heated under reflux for 1.5 hours. The mixture was cooled to 0° C., and a solution of 12.0 grams of p-tolualdehyde (0.1 mole) in 50 milliliters of ether was added dropwise. The reaction mixture was stirred at room temperature for 1 hour and then treated in the manner of Example I. The crude product was crystallized from ether to yield 10.7 grams of product (42%) as fine white needles, m.p. 99°-101° C. Analysis Calculated for C16H20N2O: C,74.96; H,7.86; N,10.93 Found: 75.19; 7.96; 10.88

WORKUP

后处理

  1. temperatureheated
  2. temperatureunder reflux for 1.5 hours
  3. temperatureThe mixture was cooled to 0° C.
  4. stirringThe reaction mixture was stirred at room temperature for 1 hour
  5. additiontreated in the manner of Example I
  6. customThe crude product was crystallized from ether