反応 #1571838

反応方程式

(2,2-difluoro-7-methyl-1,3-benzodioxol-4-yl)boronic acid

Intermediate 36

(2,2-difluoro-7-methyl-1,3-benzodioxol-4-yl)boronic acid

H2O2

NaOH

→

title compound

収率 58.1%

2,2-difluoro-7-methyl-1,3-benzodioxol-4-ol

収率 58.1%

溶媒

THF

反応条件

後処理

1. 1
   その他The reaction was quenched with a 2N aqueous solution of HCl
2. 2
   workup.ADDITIONdiluted with ethyl acetate
3. 3
   その他Two phases were separated
4. 4
   洗浄the organic layer was washed twice with brine
5. 5
   乾燥dried over Na2SO4
6. 6
   その他evaporated to dryness

実験手順

(2,2-difluoro-7-methyl-1,3-benzodioxol-4-yl)boronic acid (Intermediate 36, 150 mg, 1.28 mmol) was dissolved in THF (1.5 mL) and a 30% w/w aqueous solution of H2O2 (2.56 mmol) and NaOH (51 mg, 1.28 mmol) were added and the reaction mixture stirred for 2 days at room temperature. The reaction was quenched with a 2N aqueous solution of HCl and diluted with ethyl acetate. Two phases were separated and the organic layer was washed twice with brine, dried over Na2SO4 and evaporated to dryness, affording the title compound (140 mg) as yellow oil.

出典