Hydrogen Peroxide → 2,2-Difluoro-7-methyl-1,3-benzodioxol-4-ol

HRID 1484656노트

반응식

HRID 1484656 반응식
[F:1][C:2]1([F:15])[O:6][C:5]2[C:7]([CH3:14])=[CH:8][CH:9]=[C:10](B(O)O)[C:4]=2[O:3]1.[OH:16]O.[OH-].[Na+]>C1COCC1>[F:1][C:2]1([F:15])[O:6][C:5]2[C:7]([CH3:14])=[CH:8][CH:9]=[C:10]([OH:16])[C:4]=2[O:3]1

참가 물질

5

반응물 3

HCID 784Hydrogen PeroxideHCID 14798Sodium HydroxideHCID 86698459(2,2-Difluoro-7-methyl-1,3-benzodioxol-4-yl)boronic acid2회

생성물 1

HCID 679596912,2-Difluoro-7-methyl-1,3-benzodioxol-4-ol수율 58.1%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

(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.

후처리

  1. customThe reaction was quenched with a 2N aqueous solution of HCl
  2. additiondiluted with ethyl acetate
  3. customTwo phases were separated
  4. washthe organic layer was washed twice with brine
  5. dry with materialdried over Na2SO4
  6. customevaporated to dryness

출처 및 근거

ORD 기록
ord-c3ebc6fb425b4a178c9a8ac9f43d6560
출처 데이터셋
uspto-grants-2016_08
특허 번호
US09422272B2

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