3-Methoxyphenol → Dimethyl-(3-methoxyphenoxy)malonate

HRID 8605

反応式

HRID 8605 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([OH:9])[CH:6]=[CH:7][CH:8]=1.C([O-])([O-])=O.[K+].[K+].[CH3:16][O:17][C:18](=[O:25])[CH:19](Cl)[C:20]([O:22][CH3:23])=[O:21]>CC(C)=O>[CH3:16][O:17][C:18](=[O:25])[CH:19]([O:9][C:5]1[CH:6]=[CH:7][CH:8]=[C:3]([O:2][CH3:1])[CH:4]=1)[C:20]([O:22][CH3:23])=[O:21]

参加物

5

反応物 3

HCID 90073-MethoxyphenolHCID 11430Potassium CarbonateHCID 120070Dimethyl chloromalonate

生成物 1

HCID 21803851Dimethyl-(3-methoxyphenoxy)malonate

試薬・触媒・溶媒 1

HCID 180Acetone溶媒2 回

反応条件

温度
40 °C

実験手順

To a solution of 3-methoxyphenol (115 g) in acetone (1000 ml) was added K2CO3 (115 g). The suspension was stirred at 40° C. for 15 min. A solution of dimethylchloromalonate (133 ml) in acetone was added over a period of 45 min. The resulting brown suspension was stirred overnight at 70° C. Finally, the solvent was removed under reduced pressure and the residue was taken up in water (1000 ml) and extracted twice with DCM (500 ml). The combined organic layers were washed with water (500 ml), dried over Na2SO4, and evaporated to give crude dimethyl-(3-methoxyphenoxy)malonate (230 g) as an orange oil. The product was not purified any further.

後処理

  1. stirringThe resulting brown suspension was stirred overnight at 70° C
  2. customFinally, the solvent was removed under reduced pressure
  3. extractionextracted twice with DCM (500 ml)
  4. washThe combined organic layers were washed with water (500 ml)
  5. dry with materialdried over Na2SO4
  6. customevaporated

出典と根拠

ORDレコード
ord-e984f0b46860489fa5ffafd050372951
出典データセット
uspto-grants-2006_08
特許番号
US07091201B2

関連ノート

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