Water → 5-Methoxybenzofuran

HRID 1978765ノート

反応式

HRID 1978765 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([O:9][CH2:10][CH:11](OC)OC)=[CH:5][CH:4]=1.O>C1(C)C=CC=CC=1>[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]2[O:9][CH:10]=[CH:11][C:7]=2[CH:8]=1

参加物

4

反応物 2

HCID 962WaterHCID 110244p-(2,2-Dimethoxyethoxy)anisole

生成物 1

HCID 259435-Methoxybenzofuran収率 24.5%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
100 °C

実験手順

To a suspension of polyphosphoric acid (38.3 g) in toluene (400 ml) was added 4-methoxy-(2,2-dimethoxy)ethoxybenzene (38.0 g), and the mixture was stirred at 100° C. overnight and cooled. To the mixture was added water, and the mixture was separated. The organic layer was washed with 1N sodium hydroxide solution and then washed with saturated brine, and dried with magnesium sulfate. Under reduced pressure, the solvent was evaporated, and the residue was purified with silica gel column chromatography to give brown oil of 5-methoxybenzofuran (6.5 g).

後処理

  1. temperaturecooled
  2. customthe mixture was separated
  3. washThe organic layer was washed with 1N sodium hydroxide solution
  4. washwashed with saturated brine
  5. dry with materialdried with magnesium sulfate
  6. customUnder reduced pressure, the solvent was evaporated
  7. customthe residue was purified with silica gel column chromatography

出典と根拠

ORDレコード
ord-e1ba364eb10c41cda21078f2b7c2c28c
出典データセット
uspto-grants-2001_05
特許番号
US06235771B1

反応ノート

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