HRID1937097

反应详情

EQUATION

反应方程式

HRID 1937097 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

PdCl2/dppp (0.023 g, 1 mol %) is added and then o-bromobenzonitrile (0.72 g, 3.955 mmol) is added. The temperature rises from +10 to +300° C. over 15 min and then slowly falls to +250° C. After stirring for 3 hours at room temperature, the reaction mixture is hydrolysed using a 1N hydrochloric acid solution (15 ml). After extracting with ethyl ether, the organic phase is dried over potassium carbonate, filtered and then evaporated under vacuum. The oil thus formed is subsequently purified by chromatography (silica: 20 g; eluant: petroleum ether/ethyl acetate=95/5). The o-(p-tolyl)benzonitrile thus obtained is then harvested, with a yield of 96%, in the form of off-white crystals.

WORKUP

后处理

  1. customslowly falls to +250° C
  2. extractionAfter extracting with ethyl ether
  3. dry with materialthe organic phase is dried over potassium carbonate
  4. filtrationfiltered
  5. customevaporated under vacuum
  6. customThe oil thus formed
  7. customis subsequently purified by chromatography (silica: 20 g; eluant: petroleum ether/ethyl acetate=95/5)