m-Chloroperbenzoic acid → 4'-Fluoro-3-(1-methylethyl)[1,1'-biphenyl]-2-ol formate

HRID 2225795노트

반응식

HRID 2225795 반응식
ClC1C=CC=C([C:8]([O:10]O)=[O:9])C=1.[F:12][C:13]1[CH:18]=[CH:17][C:16]([C:19]2[C:20](C=O)=[C:21]([CH:25]([CH3:27])[CH3:26])[CH:22]=[CH:23][CH:24]=2)=[CH:15][CH:14]=1>ClCCl>[CH:8]([O:10][C:20]1[C:19]([C:16]2[CH:15]=[CH:14][C:13]([F:12])=[CH:18][CH:17]=2)=[CH:24][CH:23]=[CH:22][C:21]=1[CH:25]([CH3:26])[CH3:27])=[O:9]

참가 물질

4

반응물 2

HCID 70297m-Chloroperbenzoic acidHCID 190044654'-Fluoro-3-(1-methylethyl)[1,1'-biphenyl]-2-carboxaldehyde

생성물 1

HCID 190043884'-Fluoro-3-(1-methylethyl)[1,1'-biphenyl]-2-ol formate수율 66.1%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

3-Chloroperbenzoic acid (4.73 g) was added to a solution of 4'-fluoro-3-(1-methylethyl)[1,1'-biphenyl]-2-carboxaldehyde (3.55 g) in dichloromethane (100 mL) and the reaction mixture was stirred at room temperature overnight. The precipitated solids were removed by filtration and the filtrate was washed in turn with water, saturated sodium bisulfite solution, sodium bicarbonate solution and brine. After the dried (MgSO4) organic layer was evaporated, the crude product was purified by HPLC (ethyl acetate-hexane; 1:49) to afford 2.5 g of 4'-fluoro-3-(1-methylethyl)[1,1'biphenyl]-2-ol formate as a oil.

후처리

  1. customThe precipitated solids were removed by filtration
  2. washthe filtrate was washed in turn with water, saturated sodium bisulfite solution, sodium bicarbonate solution and brine
  3. dry with materialAfter the dried (MgSO4) organic layer
  4. customwas evaporated
  5. customthe crude product was purified by HPLC (ethyl acetate-hexane; 1:49)

출처 및 근거

ORD 기록
ord-4f5c1c27fdd84077a1a5a2d9f8e4387f
출처 데이터셋
uspto-grants-1994_09
특허 번호
US05344843

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