4-Bromo-2-fluorobenzaldehyde → 4-Bromo-2-methoxybenzaldehyde

HRID 338504

反応式

HRID 338504 の反応式
[Br:1][C:2]1[CH:9]=[CH:8][C:5]([CH:6]=[O:7])=[C:4](F)[CH:3]=1.[CH3:11][O-:12].[Na+]>CO>[Br:1][C:2]1[CH:9]=[CH:8][C:5]([CH:6]=[O:7])=[C:4]([O:12][CH3:11])[CH:3]=1

参加物

4

反応物 2

HCID 1435174-Bromo-2-fluorobenzaldehydeHCID 10942334Sodium Methoxide

生成物 1

HCID 110530414-Bromo-2-methoxybenzaldehyde収率 97.7%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

The mixture of 4-bromo-2-fluorobenzaldehyde (6.1 g, 0.03 mol) and sodium methoxide (1.78 g, 0.033 mol) in dry methanol (60 mL) was stirred at reflux for 16 hours. The methanol was evaporated. The residue was partitioned between DCM and water. The organic layers were dried over sodium sulfate, concentrated in vacuo to give a yellow solid, which was purified by silica gel chromatography (Petroleum ether/EtOAc=20:1 to 10:1) to give the title compound (6.3 g, 97%) as a light yellow solid.

後処理

  1. temperatureat reflux for 16 hours
  2. customThe methanol was evaporated
  3. customThe residue was partitioned between DCM and water
  4. dry with materialThe organic layers were dried over sodium sulfate
  5. concentrationconcentrated in vacuo
  6. customto give a yellow solid, which
  7. customwas purified by silica gel chromatography (Petroleum ether/EtOAc=20:1 to 10:1)

出典と根拠

ORDレコード
ord-355bd356a8c4475d89d84dbd5e6720e9
出典データセット
uspto-grants-2014_11
特許番号
US08889730B2

関連ノート

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