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3-Hydroxybenzaldehyde → 3-(Oxiran-2-ylmethoxy)benzaldehyde

HRID 1399803
ノート
印刷プレビュー

反応式

HRID 1399803 の反応式
[OH:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][CH:9]=1)[CH:5]=[O:6].[H-].[Na+].Cl[CH2:13][CH:14]1[CH2:16][O:15]1>CN(C=O)C>[O:15]1[CH2:16][CH:14]1[CH2:13][O:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][CH:9]=1)[CH:5]=[O:6]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 1013-HydroxybenzaldehydeHCID 7835EpichlorohydrinHCID 24758Sodium hydride

生成物 1

HCID 27740493-(Oxiran-2-ylmethoxy)benzaldehyde収率 75%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

To a solution of 3-hydroxybenzaldehyde (2.0 g, 16.38 mmol) in DMF (25 mL) was added NaH (60%, 982.6 mg, 24.57 mmol) at 0° C. in portions. The mixture was stirred at this temperature for 30 minutes before a solution of 2-(chloromethyl)oxirane (2.27 g, 24.57 mmol) in DMF (5 mL) was slowly added into the reaction mixture which was then allowed to reach room temperature slowly and stirred for 16 h. The solvent was removed by concentration and the residue dissolved in ethyl acetate and washed with water. T the separated organic layer was dried over sodium sulfate, filtered and concentrated. The crude product was then purified by column chromatography. (2.2 g, yield 75%) MS (ESI+) e/z: 179.1 [M+1]+.

後処理

  1. additionwas slowly added into the reaction mixture which
  2. customto reach room temperature
  3. customThe solvent was removed by concentration
  4. dissolutionthe residue dissolved in ethyl acetate
  5. washwashed with water
  6. dry with materialT the separated organic layer was dried over sodium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated
  9. customThe crude product was then purified by column chromatography

出典と根拠

ORDレコード
ord-3f3842823b354d9185857afab647e5eb
出典データセット
uspto-grants-2014_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08906900B2

反応ノート

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