Water → 4-Bromo-1-naphthaldehyde

HRID 388367

反応式

HRID 388367 の反応式
[C:1](=[O:4])(O)[O-].[Na+].[Br:6][C:7]1[C:16]2[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=2)[C:10](CBr)=[CH:9][CH:8]=1.O>CS(C)=O>[Br:6][C:7]1[C:16]2[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=2)[C:10]([CH:1]=[O:4])=[CH:9][CH:8]=1

参加物

5

反応物 3

HCID 962WaterHCID 516892Sodium BicarbonateHCID 127491471-Bromo-4-(bromomethyl)naphthalene

生成物 1

HCID 46404134-Bromo-1-naphthaldehyde

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

反応条件

温度
95 °C

実験手順

Sodium bicarbonate (1.4 g) is added to a solution of crude 1-bromo-4-bromomethyl-naphthalene (2.5 g) in DMSO (25 ml). The reaction is stirred for 3 h at 95° C. and cooled down to room temperature. Water is added and the mixture is extracted with ethyl acetate. The organic phase is dried over MgSO4 and concentrated in vacuo. The crude product is purified on a semi-preparative HPLC to yield 4-bromo-naphthalene-1-carbaldehyde as colorless crystals.

後処理

  1. temperaturecooled down to room temperature
  2. extractionthe mixture is extracted with ethyl acetate
  3. dry with materialThe organic phase is dried over MgSO4
  4. concentrationconcentrated in vacuo
  5. customThe crude product is purified on a semi-preparative HPLC

出典と根拠

ORDレコード
ord-554be38d43774d25bd92901008251605
出典データセット
uspto-grants-2013_02
特許番号
US08377942B2

関連ノート

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