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HRID1108516

反应详情

EQUATION

反应方程式

HRID 1108516 的结构方程式

REACTANTS

反应物

3
结构：O=S(=O)(O)O
HCID1118

Sulfuric acid

H2O4S

结构：Clc1ccc(Br)cc1
HCID7806

p-Bromoclorobenzene

C6H4BrCl

结构：C1CCOC1.C[Si](C)(C)N(c1cccc([Mg]Cl)c1)[Si](C)(C)C
HCID178420688

未命名化合物

PRODUCTS

生成物

1
结构：C[Si](C)(C)N(c1cccc(-c2ccc(Cl)cc2)c1)[Si](C)(C)C
HCID15451739

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

2
结构：Cl[Pd]Cl.[Fe+2].c1ccc(P(c2ccccc2)[c-]2cccc2)cc1.c1ccc(P(c2ccccc2)[c-]2cccc2)cc1
催化剂HCID178418228

Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+)

C34H28Cl2FeP2Pd

结构：C1CCOC1
溶剂HCID8028

Tetrahydrofuran

C4H8O

PROCEDURE

实验过程

0.5 mol of a 25% strength by weight 3-bis(trimethylsilyl)aminophenyl-magnesium chloride/THF solution is added dropwise in the course of 30 minutes to a boiling solution of 0.5 mol of 1,4-bromochlorobenzene and 0.0025 g of Pd(dppf)Cl2 *CH2Cl2 in 100 ml THF. After stirring under reflux for four hours, the mixture is hydrolyzed with dilute sulfuric acid (conversion 99%, selectivity 97%). The organic phase is freed from the solvent by distillation. The crude 4-chloro-3'-bis(trimethylsilyl)aminobiphenyl thus obtained is recrystallized from isopropanol.

WORKUP

后处理

  1. temperatureunder reflux for four hours
  2. distillationThe organic phase is freed from the solvent by distillation