1,2,3-Trimethoxybenzene → 5-Oxo-5-(2,3,4-trimethoxy-phenyl)-pentanoic acid methyl ester

HRID 33953

반응식

HRID 33953 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[C:5]([O:9][CH3:10])[C:4]=1[O:11][CH3:12].[CH3:13][O:14][C:15](=[O:22])[CH2:16][CH2:17][CH2:18][C:19]([O-])=[O:20]>>[CH3:13][O:14][C:15](=[O:22])[CH2:16][CH2:17][CH2:18][C:19](=[O:20])[C:6]1[CH:7]=[CH:8][C:3]([O:2][CH3:1])=[C:4]([O:11][CH3:12])[C:5]=1[O:9][CH3:10]

참가 물질

3

반응물 2

HCID 124621,2,3-TrimethoxybenzeneHCID 69931945-Methoxy-5-oxopentanoate

생성물 1

HCID 689200075-Oxo-5-(2,3,4-trimethoxy-phenyl)-pentanoic acid methyl ester수율 77%

반응 조건

온도
45 °C

실험 절차

75 g of polyphosphoric acid (Acros) was charged in a 250 mL round bottom flask, followed by addition of 1,2,3-trimethoxybenzene (5.0 g, 29.73 mmol), and mono-methylglutarate (6.516 g, 44.60 mmol). The reaction mixture was stirred mechanically for 2.5 h at 45° C. The reaction mixture was then poured into a 1000 mL beaker containing around 250 mL of ice, and stirred well until all the product precipitated out. The tan colored product was then filtered and washed with water and dried under vacuum. No, purification required at this stage. 6.78 g (77%) of product was obtained, which was pure by NMR.

후처리

  1. additionThe reaction mixture was then poured into a 1000 mL beaker
  2. stirringstirred well until all the product
  3. customprecipitated out
  4. filtrationThe tan colored product was then filtered
  5. washwashed with water
  6. customdried under vacuum
  7. customNo, purification

출처 및 근거

ORD 기록
ord-31bb2fbdf8ae4a799762b97d126b8f44
출처 데이터셋
uspto-grants-2008_09
특허 번호
US07429681B2

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