Potassium Carbonate → Methyl 2-(4-methoxybenzyloxy)-5-methylbenzoate

HRID 660787

反応式

HRID 660787 の反応式
[CH3:1][O:2][C:3](=[O:12])[C:4]1[CH:9]=[C:8]([CH3:10])[CH:7]=[CH:6][C:5]=1[OH:11].[CH3:13][O:14][C:15]1[CH:22]=[CH:21][C:18]([CH2:19]Cl)=[CH:17][CH:16]=1.C([O-])([O-])=O.[K+].[K+]>CN(C=O)C.CCOC(C)=O>[CH3:1][O:2][C:3](=[O:12])[C:4]1[CH:9]=[C:8]([CH3:10])[CH:7]=[CH:6][C:5]=1[O:11][CH2:19][C:18]1[CH:21]=[CH:22][C:15]([O:14][CH3:13])=[CH:16][CH:17]=1

参加物

6

反応物 3

HCID 11430Potassium CarbonateHCID 699934-Methyloxybenzyl chlorideHCID 89802Methyl 5-methylsalicylate

生成物 1

HCID 66756631Methyl 2-(4-methoxybenzyloxy)-5-methylbenzoate

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
60 °C

実験手順

A mixture of 2-hydroxy-5-methylbenzoic acid methyl ester (4.98 g, 30 mmol), 4-methoxybenzyl chloride (4.69 g, 30 mmol) and K2CO3 (4.55 g, 33 mmol) in DMF (50 mL) is stirred at 60° C. for 48 h. The mixture is diluted with EtOAc and washed with 1N HCl and brine then the organic phase is dried over magnesium sulfate. The solvent is removed under reduced pressure and the residue is purified by column chromatography using a gradient of 0-100% EtOAc/hexane as eluent to give the title compound as a colorless oil.

後処理

  1. washwashed with 1N HCl and brine
  2. dry with materialthe organic phase is dried over magnesium sulfate
  3. customThe solvent is removed under reduced pressure
  4. customthe residue is purified by column chromatography

出典と根拠

ORDレコード
ord-df74d21babdf4d7fb4b3e37e2a9c428e
出典データセット
uspto-grants-2011_12
特許番号
US08084448B2

関連ノート

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