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HRID1266711

反应详情

EQUATION

反应方程式

HRID 1266711 的结构方程式

REACTANTS

反应物

3
结构：c1c[nH]cn1
HCID795

Imidazole

C3H4N2

结构：CC(C)(C)[Si](Cl)(c1ccccc1)c1ccccc1
HCID94078

Silane, chloro(1,1-dimethylethyl)diphenyl-

C16H19ClSi

结构：CC(C)(C)[Si](C)(C)Oc1ccc(F)c(O)c1
HCID13861698

未命名化合物

PRODUCTS

生成物

1
结构：CC(C)(C)[Si](C)(C)Oc1ccc(F)c(O[Si](c2ccccc2)(c2ccccc2)C(C)(C)C)c1
HCID18551826

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

1
结构：CN(C)C=O
溶剂HCID6228

N,N-Dimethylformamide

C3H7NO

PROCEDURE

实验过程

A solution of 53.0 g 5-(tert-butyl-dimethyl-silanyloxy)-2-fluoro-phenol (M. Kawase, A. K. Sinhababu, R. T. Borchardt, Chem. Pharm. Bull. (1990),38, 2939) in 120 ml DMF was cooled to 0° C. Within 15 min 61.6 ml tert-butyldiphenylsilyl chloride were added. Then 16.4 g imidazole were added portionwise. The suspension was stirred overnight, then quenched with 150 ml H2O at 0° C. The crude product was isolated by extraction with hexanes and purified by chromatography on silica gel (hexanes) to yield 88.9 g of 4-(tert-butyl-dimethyl-silanyloxy)-2-(tert-butyl-diphenyl-silanyloxy)-fluorobenzene as colorless liquid.

WORKUP

后处理

  1. customquenched with 150 ml H2O at 0° C
  2. customThe crude product was isolated by extraction with hexanes
  3. custompurified by chromatography on silica gel (hexanes)