HRID263219

反应详情

EQUATION

反应方程式

HRID 263219 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Concentrated hydrochloric acid (8.1 ml) was added dropwise over 10 minutes to a mixture of 1-(p-methoxy)phenoxy-3-methylbut-2-ene (VI; R=CH2OC6H4.OCH3, R1 =R2 =CH3) (16.05 g) and amyl nitrite (12.1 ml) in glacial acetic acid (16.2 ml) at -5° to 0° (ice-salt bath). After a further 1 hour at -5° to 0°, the mixture was filtered. The solid so obtained was washed with acetone and recrystallised from acetone to give the nitrosochloride (V) (4.87 g, yield 22%) as pale yellow crystals, m.p. 123° (decomp.).

WORKUP

后处理

  1. filtrationthe mixture was filtered
  2. customThe solid so obtained
  3. washwas washed with acetone
  4. customrecrystallised from acetone