3,4-二硝基氯苯 → ethyl P-methyl-2-nitro-5-chlorophenylphosphinate

HRID 463560

反应方程式

HRID 463560 反应方程式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[C:4]([N+]([O-])=O)[CH:3]=1.[CH3:14][P:15]([O:19]CC)[O:16][CH2:17][CH3:18]>C(#N)C>[CH3:14][P:15]([C:4]1[CH:3]=[C:2]([Cl:1])[CH:7]=[CH:6][C:5]=1[N+:8]([O-:10])=[O:9])(=[O:19])[O:16][CH2:17][CH3:18]

参与物

4

反应物 2

HCID 330973,4-二硝基氯苯HCID 85063甲基二乙氧基膦

产物 1

HCID 53860251ethyl P-methyl-2-nitro-5-chlorophenylphosphinate

试剂、催化剂与溶剂 1

HCID 6342乙腈溶剂

实验过程

To 4-chloro-1,2-dinitrobenzene (13.2 g, 65.0 mmol) dissolved in acetonitrile (150 ml) is added, dropwise, diethyl methylphosphonite (16.0 g, 117.6 mmol). The mixture is stirred at RT for 20 hours, after which it is concentrated. The crude product is purified by column chromatography (developing with 50% ethyl acetate/hexane) to yield ethyl P-methyl-2-nitro-5-chlorophenylphosphinate.

后处理

  1. additionis added
  2. concentrationafter which it is concentrated
  3. customThe crude product is purified by column chromatography (developing with 50% ethyl acetate/hexane)

来源与证据

ORD记录
ord-cd5e6dca7b5048fab9a1583e2647bcfa
来源数据集
uspto-grants-1985_05
专利号
US04520197

关联笔记

加载中…