HRID375520

反应详情

EQUATION

反应方程式

HRID 375520 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
130 °C

PROCEDURE

实验过程

The 2-amino-3-cyanofuran produced in the preceding step was combined with 4.2 mL of triethylorthoformate, and 0.5 mL of acetic anhydride, and the mixture was heated to 130° C. for two hours. Then was added 1.8 g of sodium acetate and 3 g of 2-(4-methoxyphenyl)ethylamine, followed by 3 mL of acetic acid. The resulting mixture was heated for two hours at 130°-138° C., then cooled and diluted with water. The product was extracted with large volumes of ether. The ether extracts were combined, washed with water, dried over magnesium sulfate, and concentrated. The residue was recrystallized from ether and petroleum ether. Yield 0.65 g. M.P. 135°-136° C.

WORKUP

后处理

  1. temperatureThe resulting mixture was heated for two hours at 130°-138° C.
  2. temperaturecooled
  3. extractionThe product was extracted with large volumes of ether
  4. washwashed with water
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated
  7. customThe residue was recrystallized from ether and petroleum ether