反応 #1562968

反応方程式

7-(5,5-dimethyl-[1,3,2]dioxaborinan-2-yl)-2,2-difluoro-benzo[1,3]dioxole-5-carboxylic acid methyl ester

H2O2

→

title compound

2,2-Difluoro-7-hydroxy-benzo[1,3]dioxole-5-carboxylic acid methyl ester

溶媒

methanol

反応条件

後処理

1. 1
   workup.ADDITIONadded
2. 2
   濃縮The reaction mixture was then concentrated to 20 ml and 100 ml of water and 100 ml of a saturated aqueous NaCl-solution
3. 3
   workup.ADDITIONadded
4. 4
   抽出The reaction mixture was then extracted three times
5. 5
   その他dried
6. 6
   その他evaporated

実験手順

6.0 g of 7-(5,5-dimethyl-[1,3,2]dioxaborinan-2-yl)-2,2-difluoro-benzo[1,3]dioxole-5-carboxylic acid methyl ester were dissolved using 200 ml of methanol and 30 ml of a 33% aqueous solution of H2O2 added. Stirring was continued for 30 minutes at room temperature. The reaction mixture was then concentrated to 20 ml and 100 ml of water and 100 ml of a saturated aqueous NaCl-solution added. The reaction mixture was then extracted three times using 100 ml of CH2Cl2 each, dried using MgSO4, and evaporated. Chromatography on silica gel using EA/HEP 1:4 yielded 1.8 g of the title compound, colorless oil.

出典