HRID435043

反应详情

EQUATION

反应方程式

HRID 435043 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Sixty-nine grams (0.5 mole) of m-nitroaniline and 76 grams (g.) (0.52 mole) of 2,2-dimethylsuccinic acid were mixed with 200 milliliters (ml.) of xylene and heated to reflux until approximately 20 ml. of water was removed in a modified Dean Stark apparatus. On cooling, the product crystallized from solution. The mixture was diluted with 300 ml. of ether, the solid filtered off, washed with an additional 100 ml. of ether and dried. Yield was 117.5 g. of a product having a melting point (m.p.) of 134°-134.5° C. The product was identified as the title compound by analysis of infrared spectra.

WORKUP

后处理

  1. temperatureheated
  2. temperatureto reflux until approximately 20 ml
  3. customof water was removed in a modified Dean Stark apparatus
  4. temperatureOn cooling
  5. customthe product crystallized from solution
  6. additionThe mixture was diluted with 300 ml
  7. filtrationof ether, the solid filtered off
  8. washwashed with an additional 100 ml
  9. dry with materialof ether and dried
  10. customa melting point (m.p.) of 134°-134.5° C