تفاعل #614838

معادلة التفاعل

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

Intermediate 196

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

H2O2

NaOH

→

title compound

المردود 58.1%

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

المردود 58.1%

المذيبات

THF

ظروف التفاعل

المعالجة

1. 1
   أخرىThe reaction was quenched with a 2N aqueous solution of HCl
2. 2
   workup.ADDITIONdiluted with ethyl acetate
3. 3
   أخرىTwo phases were separated
4. 4
   غسيلthe organic layer was washed twice with brine
5. 5
   تجفيفdried over Na2SO4
6. 6
   أخرىevaporated to dryness

الإجراء التجريبي

(2,2-difluoro-7-methyl-1,3-benzodioxol-4-yl)boronic acid (Intermediate 196, 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.

المصدر