Dopac → 3,4-Diethoxyphenylacetic acid

HRID 1007372

反応式

HRID 1007372 の反応式
[OH:1][C:2]1[CH:3]=[C:4]([CH2:9][C:10]([OH:12])=[O:11])[CH:5]=[CH:6][C:7]=1[OH:8].O.O.O.O.O.O.O.O.[OH-].[Ba+2].[OH-].S([O-])(O)(=O)=O.[K+].[C:30](OCC)(=O)[CH3:31].[CH2:36](OS(OCC)(=O)=O)[CH3:37]>O>[CH2:30]([O:1][C:2]1[CH:3]=[C:4]([CH2:9][C:10]([OH:12])=[O:11])[CH:5]=[CH:6][C:7]=1[O:8][CH2:36][CH3:37])[CH3:31]

参加物

7

反応物 5

HCID 547DopacHCID 6163Diethyl SulfateHCID 8857Ethyl AcetateHCID 516920Potassium bisulfateHCID 17749109Barium hydroxide, octahydrate

生成物 1

HCID 5798133,4-Diethoxyphenylacetic acid

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
40 °C

実験手順

0.8 g of 3,4-dihydroxy-phenylacetic acid and 6.9 g of barium hydroxide octahydrate are dissolved in 50 ml of water and at ambient temperature 2.9 ml of diethylsulphate are added dropwise. The solution is stirred for 2 hours at ambient temperature and for 2 hours at 40° C. After this time the solution is acidified with saturated potassium hydrogen sulphate solution, mixed with ethyl acetate and the suspension is filtered through Celite. The phases are separated and the ethyl acetate phase is dried over sodium sulphate and concentrated by evaporation. The residue obtained is purified through a silica gel column with toluene/ethyl acetate/ethanol (4:2:1) as eluant.

後処理

  1. additionare added dropwise
  2. filtrationthe suspension is filtered through Celite
  3. customThe phases are separated
  4. dry with materialthe ethyl acetate phase is dried over sodium sulphate
  5. concentrationconcentrated by evaporation
  6. customThe residue obtained
  7. customis purified through a silica gel column with toluene/ethyl acetate/ethanol (4:2:1) as eluant

出典と根拠

ORDレコード
ord-4b67fc642c024da69356a00d8d3e23ff
出典データセット
uspto-grants-2004_09
特許番号
US06794395B1

関連ノート

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