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HRID506841

反应详情

EQUATION

反应方程式

HRID 506841 的结构方程式

REACTANTS

反应物

4
结构：COC(C)(C)C
HCID15413

Methyl tert-butyl ether

C5H12O

结构：CCCC[N+](CCCC)(CCCC)CCCC.[F-]
HCID2724141

Tetra-n-butylammonium fluoride

C16H36FN

结构：C[Si](C)(C)C(C(N)=O)[Si](C)(C)C
HCID11708267

Bistrimethylsilylacetamid

C8H21NOSi2

结构：COc1ccc(C(Nc2ccc([N+](=O)[O-])cc2)C(CCC(O[Si](C)(C)C(C)(C)C)c2ccccc2)C(=O)N2C(=O)OCC2c2ccccc2)cc1
HCID68640083

未命名化合物

PRODUCTS

生成物

1
结构：COc1cccc(C2C(CCC(O[Si](C)(C)C(C)(C)C)c3ccccc3)C(=O)N2c2ccc([N+](=O)[O-])cc2)c1
HCID68639713

未命名化合物

收率 70%

AUXILIARIES

试剂、催化剂与溶剂

1
结构：CC(=O)O
溶剂HCID176

Acetic Acid

C2H4O2

PROCEDURE

实验过程

A mixture comprising 6.1 g (8.6 mmol) of product 3, 7.3 ml of bistrimethylsilylacetamid, 0.5 g of Tetrabutylammoniumfluorid and 100 ml of tert-butylmethylether is stirred under a argon atmosphere for 10 h at room temperature. After finishing of the reaction 5 ml of acetic acid are added slowly by cooling with ice and evaporated. The residue is separated by chromatography on silica gel (ethylacetate/heptane=1/2). 3.3 g (70%) of product 4 is obtained in form of a light yellow compound in solid form: C31H38N2O5Si (546.74) MS (ESI+) 547.3 (M+H+).

WORKUP

后处理

  1. additionare added slowly
  2. temperatureby cooling with ice
  3. customevaporated
  4. customThe residue is separated by chromatography on silica gel (ethylacetate/heptane=1/2)