反应 #1435684

ord-0a6bb4abb0ea46b188b38626ba29424e

反应方程式

[Na+].[OH-]
sodium hydroxide
COc1c(C)cc(NC(=O)OCCCl)cc1NC(=O)OCCCl
bis(2-chloroethyl) (4-methoxy-5-methyl-1,3-phenylene)biscarbamate
Cl
hydrochloric acid
COc1c(C)cc(N2CCOC2=O)cc1N1CCOC1=O
3,3′-(4-methoxy-5-methyl-1,3-phenylene)bis(1,3-oxazolidin-2-one)

溶剂

反应条件

温度
45°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.STIRRINGAfter stirring overnight at room temperature
  2. 2
    workup.ADDITIONthe mixture was poured onto ice
  3. 3
    过滤The precipitated product was filtered off with suction
  4. 4
    其他dried overnight under reduced pressure

实验过程

200 ml of sodium hydroxide solution (20% strength) were initially introduced and heated to 45° C. Subsequently, 59 g of bis(2-chloroethyl) (4-methoxy-5-methyl-1,3-phenylene)biscarbamate were added in portions and the mixture was diluted with 200 ml of dioxane. The mixture was after-stirred for a further 2 h at 45° C. After stirring overnight at room temperature, the mixture was poured onto ice, and the mixture was neutralized with hydrochloric acid. The precipitated product was filtered off with suction and dried overnight under reduced pressure.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07211119B2uspto-grants-2007_05