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

HRID 33958

反応式

HRID 33958 の反応式
[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].[C:13]([O:20][CH3:21])(=[O:19])[CH2:14][CH2:15][C:16]([O-])=[O:17]>>[CH3:21][O:20][C:13](=[O:19])[CH2:14][CH2:15][C:16](=[O:17])[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]

参加物

3

反応物 2

HCID 124621,2,3-TrimethoxybenzeneHCID 6930703Mono-Methyl Succinate

生成物 1

HCID 447204584-Oxo-4-(2,3,4-trimethoxy-phenyl)-butyric acid methyl ester収率 72.7%

反応条件

温度
45 °C

実験手順

A mixture of 75 g of polyphosphoric acid (Acros), 1,2,3-trimethoxybenzene (5.0 g, 29.73 mmol), and mono-methyl succinate (5.9 g, 44.59 mmol) were mechanically stirred at 45° C. for 2.5 h. The reaction mixture was then poured into a 1000 mL beaker containing round 250 mL of ice, and stirred well until all the product was precipitated out. The tan colored product was then filtered and washed with water and dried under vacuum. 6.1 g (72%) of 55 was obtained, which was pure by NMR.

後処理

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

出典と根拠

ORDレコード
ord-bdb5c2efb4434099bfacdae154ddb13a
出典データセット
uspto-grants-2008_09
特許番号
US07429681B2

関連ノート

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