反应 #5635

反应方程式

Compound 15

6-dodecyl-6-(2-hydroxybenzyl)-13,13-dimethyl-1,4,8,11-tetraoxacyclotetradecane

2-methylsulfonyl-4-nitrophenyldiazonium hexafluorophosphate

→

Compound 16

收率 4.9%

6-Dodecyl-6-[2-hydroxy-5-(2-methylsulfonyl-4-nitrophenylazo)benzyl]-13,13-dimethyl-1,4,8,11-tetraoxacyclotetradecane

收率 4.9%

溶剂

acetic acid

water

tetrahydrofuran

反应条件

后处理

1. 1
   萃取The product was extracted into ethyl acetate
2. 2
   其他isolated by silica gel chromatography

实验过程

To a solution of 3.1 g (6.1 mmol) of Compound 15 in 50 cc acetic acid at 5° C. was added a solution of 3.0 g (8.0 mmol) of 2-methylsulfonyl-4-nitrophenyldiazonium hexafluorophosphate in 25 cc water and 75 cc tetrahydrofuran. The suspension was stirred at room temperature for 16 hours. The product was extracted into ethyl acetate and isolated by silica gel chromatography yielding 0.22 g (4.7%) of Compound 16. The 1H NMR spectrum is consistent with the assigned structure.

来源