HRID463963

反应详情

EQUATION

反应方程式

HRID 463963 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Benzil 63.1 grams (0.3 mole) along with 30 grams (0.3 mole) of cyanoacetohydrazide in 200 mls of dimethylformamide was heated at 110° C. for five hours. The solution was cooled and the precipitant solid was filtered and washed with ethyl alcohol. The filtrate was vacuum distilled and the residual solid was washed with ethyl alcohol and filtered. There was isolated 74.5 grams, a 95% yield, of a solid which melted at 280°-281° C. Calculated for C17H11N3O, C, 74.7; H, 4.1; N, 15.4. Found: C, 74.4; H, 4.16; N, 15.2. The infrared spectra showed the nitrile at 4.5μ; the ##STR57## band for an amide at 6.0μ.

WORKUP

后处理

  1. temperatureThe solution was cooled
  2. filtrationthe precipitant solid was filtered
  3. washwashed with ethyl alcohol
  4. distillationdistilled
  5. washthe residual solid was washed with ethyl alcohol
  6. filtrationfiltered
  7. customThere was isolated 74.5 grams