HRID375501

反应详情

EQUATION

反应方程式

HRID 375501 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 1,2-dicyano-3-nitrobenzene (2.77 parts) and sodium phenoxide (2.79 parts) in dimethylformamide (50 parts) was stirred at 120° C. for 2 hours. The reaction mixture was poured into water and extracted with diethyl ether (100 parts). The diethyl ether extract was washed with 5% aqueous potassium hydroxide solution (2×200 parts) and water (2×200 parts) and the diethyl ether was removed under reduced pressure to leave a solid. Recrystallisation of the solid from a 1:1 diethyl ether:petroleum spirit (b.pt.60°-80° C.) gave 1,2-dicyano-3-phenoxybenzene (2.1 parts, 60%) as a pale green solid, m.pt.110°-112° C.

WORKUP

后处理

  1. extractionextracted with diethyl ether (100 parts)
  2. extractionThe diethyl ether extract
  3. washwas washed with 5% aqueous potassium hydroxide solution (2×200 parts) and water (2×200 parts)
  4. customthe diethyl ether was removed under reduced pressure
  5. customto leave a solid
  6. customRecrystallisation of the solid from a 1:1 diethyl ether