Triphenylphosphine → HCID 67324702, 화합물

HRID 1028981

반응식

HRID 1028981 반응식
[Br:1][C:2]1[C:7]([CH3:8])=[CH:6][CH:5]=[CH:4][C:3]=1[CH2:9][OH:10].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[Cl:30][C:31]1[CH:36]=[CH:35][C:34]([C:37]([F:40])([F:39])[F:38])=[CH:33][C:32]=1O.N(C(OCC)=O)=NC(OCC)=O>C(Cl)Cl>[Br:1][C:2]1[C:7]([CH3:8])=[CH:6][CH:5]=[CH:4][C:3]=1[CH2:9][O:10][C:32]1[CH:33]=[C:34]([C:37]([F:39])([F:40])[F:38])[CH:35]=[CH:36][C:31]=1[Cl:30]

참가 물질

6

반응물 4

HCID 11776TriphenylphosphineHCID 123498Phenol, 2-chloro-5-(trifluoromethyl)-HCID 220568ethyl N-ethoxycarbonyliminocarbamateHCID 52987706(2-Bromo-3-methylphenyl)methanol

생성물 1

HCID 67324702HCID 67324702, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of (2-bromo-3-methylphenyl)methanol (0.5 g, 2.49 mmol), triphenylphosphine (1.31 g, 4.97 mmol) and 2-chloro-5-(trifluoromethyl)phenol (0.37 mL, 2.74 mmol) in DCM (12.4 mL) at 0° C. was added diethyl azodicarboxylate (1.97 mL, 4.97 mmol) and the reaction warmed to RT for 30 min. The reaction was quenched with water and the aqueous layer was extracted with EtOAc. The organic layer was then washed with water and brine (3× ea.), dried over Na2SO4 and concentrated in vacuo. The crude material was purified by column chromatography (0-50% Hexene/EtOAc) to afford 2-bromo-1-((2-chloro-5-(trifluoromethyl)phenoxy)methyl)-3-methylbenzene as a clear oil.

후처리

  1. customThe reaction was quenched with water
  2. extractionthe aqueous layer was extracted with EtOAc
  3. washThe organic layer was then washed with water and brine (3× ea.)
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated in vacuo
  6. customThe crude material was purified by column chromatography (0-50% Hexene/EtOAc)

출처 및 근거

ORD 기록
ord-e3f1a608aece4bdfb61e9b6616cbd648
출처 데이터셋
uspto-grants-2014_05
특허 번호
US08735384B2

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