反応 #5635

反応方程式

Compound 15

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

2-methylsulfonyl-4-nitrophenyldiazonium hexafluorophosphate

→

Compound 16

収率 4.9%

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

収率 4.9%

溶媒

acetic acid

water

tetrahydrofuran

反応条件

後処理

1. 1
   抽出The product was extracted into ethyl acetate
2. 2
   その他isolated by silica gel chromatography

実験手順

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.

出典