HRID437532

反应详情

EQUATION

反应方程式

HRID 437532 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 0.15 mole each of p-chlorophenylurea, phenyl diphenylphosphinite, and n-butyraldehyde in 150g of toluene is warmed at reflux for 5.5 hr, giving a reaction mixture having a 31P nmr signal only at 3136.8 ppm. When the toluene is removed at reduced pressure, the residue solidifies. Recrystallization of a portion from benzene gives a white solid: mp 275°-278° C; 31P nmr -37.4 ppm; 1H nmr δ9.1 (s, 1, NHC6H4Cl), 6.4-8.1 (m, 15, aryl and CHNH), 5.1 (m, 1, PCH), 0.6-2.0 (m, 7, CH2CH2CH3).

WORKUP

后处理

  1. temperatureis warmed
  2. temperatureat reflux for 5.5 hr
  3. customgiving a reaction mixture
  4. customWhen the toluene is removed at reduced pressure
  5. customRecrystallization of a portion from benzene
  6. customgives a white solid