Methanol → Methyl 4-(1-methoxyethyl)benzoate

HRID 1479726

反応式

HRID 1479726 の反応式
[CH3:1]O.[Bi](Br)(Br)Br.[OH:7][CH:8]([C:10]1[CH:19]=[CH:18][C:13]([C:14]([O:16][CH3:17])=[O:15])=[CH:12][CH:11]=1)[CH3:9]>ClC(Cl)(Cl)Cl>[CH3:17][O:16][C:14](=[O:15])[C:13]1[CH:18]=[CH:19][C:10]([CH:8]([O:7][CH3:1])[CH3:9])=[CH:11][CH:12]=1

参加物

5

反応物 3

HCID 887MethanolHCID 82232bismuth(III) bromideHCID 586417Methyl 4-(1-hydroxyethyl)benzoate

生成物 1

HCID 14597192Methyl 4-(1-methoxyethyl)benzoate収率 57%

試薬・触媒・溶媒 1

HCID 5943Carbon Tetrachloride溶媒

実験手順

To the solution of methanol (53 mg, 1.67 mmol) in perchloromethane (80 mL) was added bismuth (III) bromide (743 mg, 1.67 mmol), the mixture was stirred for 30 minutes at room temperature, the methyl 4-(1-hydroxyethyl)benzoate (300 mg, 1.67 mmol) was added, the mixture was stirred at room temperature for 12 hours. Then the mixture was concentrated and purified by column chromatography (silica gel, Petroleum ether/ethyl acetate=20:1) to give methyl-4-(1-methoxyethyl)benzoate (185 mg, 57%), as oil.

後処理

  1. stirringthe mixture was stirred at room temperature for 12 hours
  2. concentrationThen the mixture was concentrated
  3. custompurified by column chromatography (silica gel, Petroleum ether/ethyl acetate=20:1)

出典と根拠

ORDレコード
ord-d2d43a9475f9494c8b9dcb738c8fe8bd
出典データセット
uspto-grants-2016_08
特許番号
US09409865B2

関連ノート

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