Phenol → HCID 67333442, 화합물

HRID 1669642

반응식

HRID 1669642 반응식
[F:1][C:2]([F:11])([F:10])[CH:3]1[CH2:8][CH2:7][C:6](=O)[CH2:5][CH2:4]1.[C:12]1([OH:18])[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1>Cl.CCOC(C)=O.C([O-])(O)=O.[Na+]>[F:1][C:2]([F:11])([F:10])[CH:3]1[CH2:8][CH2:7][C:6]([C:15]2[CH:16]=[CH:17][C:12]([OH:18])=[CH:13][CH:14]=2)([C:15]2[CH:16]=[CH:17][C:12]([OH:18])=[CH:13][CH:14]=2)[CH2:5][CH2:4]1

참가 물질

6

반응물 2

HCID 996PhenolHCID 27774914-(Trifluoromethyl)cyclohexanone

생성물 1

HCID 67333442HCID 67333442, 화합물

시약·촉매·용매 3

HCID 313Hydrochloric Acid용매HCID 8857Ethyl Acetate용매HCID 516892Sodium Bicarbonate용매

실험 절차

A solution of 4-(trifluoromethyl)cyclohexanone (1.13 g, 6.8 mmol) and phenol (2.01 g, 21.4 mmol) in 3 mL of concentrated HCl (aq) was stirred at 40° C. for 18 h. The reaction mixture was diluted with EtOAc and saturated aqueous NaHCO3 was slowly added. The organic layer was collected and the aqueous layer was extracted twice with EtOAc. The combined organic layers were concentrated under reduced pressure. The residue was purified by flash chromatography on silica gel eluting with a gradient of 0% to 40% EtOAc/hexanes over 10 column volumes, then 40% to 100% EtOAc/hexanes over 5 column volumes, affording the title compound as a white solid.

후처리

  1. additionwas slowly added
  2. customThe organic layer was collected
  3. extractionthe aqueous layer was extracted twice with EtOAc
  4. concentrationThe combined organic layers were concentrated under reduced pressure
  5. customThe residue was purified by flash chromatography on silica gel eluting with a gradient of 0% to 40% EtOAc/hexanes over 10 column volumes

출처 및 근거

ORD 기록
ord-66dcd8f751764dc8aef01be8a59c9e70
출처 데이터셋
uspto-grants-2011_08
특허 번호
US07989472B2

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