Water → Ethyl 2-(3,5-dimethylphenoxy)acetate

HRID 628151노트

반응식

HRID 628151 반응식
[CH3:1][C:2]1[CH:3]=[C:4]([OH:9])[CH:5]=[C:6]([CH3:8])[CH:7]=1.Br[CH2:11][C:12]([O:14][CH2:15][CH3:16])=[O:13].C([O-])([O-])=O.[K+].[K+].O>CC#N>[CH3:1][C:2]1[CH:3]=[C:4]([CH:5]=[C:6]([CH3:8])[CH:7]=1)[O:9][CH2:11][C:12]([O:14][CH2:15][CH3:16])=[O:13]

참가 물질

6

반응물 4

HCID 962WaterHCID 7748Ethyl bromoacetateHCID 79483,5-DimethylphenolHCID 11430Potassium Carbonate

생성물 1

HCID 7018365Ethyl 2-(3,5-dimethylphenoxy)acetate

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

Referring to FIG. 37, to a solution of 3,5-dimethylphenol (10 g, 82 mmol) in CH3CN (150 mL) were added ethyl 2-bromoacetate (14.9 g, 90 mmol) and K2CO3 (16.9 g, 123 mmol). The reaction mixture was stirred overnight at room temperature. The mixture was poured into water (200 mL) and the resulting mixture was extracted with ethyl acetate (150 mL×2). The combined extracts were washed with brine, dried over anhydrous Na2SO4 and concentrated under reduced pressure to give product as a yellow oil, which was used in the next step without further purification (19 g); 1H NMR (CDCl3, 300 MHz): δ 6.13 (s, 1H), 6.11 (s, 2H), 4.59 (s, 2H), 4.30 (q, J=7.2 Hz, 2H), 3.77 (s, 6H), 1.31 (t, J=7.2 Hz, 3H).

후처리

  1. extractionthe resulting mixture was extracted with ethyl acetate (150 mL×2)
  2. washThe combined extracts were washed with brine
  3. dry with materialdried over anhydrous Na2SO4
  4. concentrationconcentrated under reduced pressure
  5. customto give product as a yellow oil, which
  6. customwas used in the next step without further purification (19 g)

출처 및 근거

ORD 기록
ord-cf674342a19f4d8cb92de2e0b63ea601
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09309283B2

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