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[2-(Bromomethyl)-3-chlorophenyl]methanol → 2-(Bromomethyl)-3-chlorobenzaldehyde

HRID 446028
ノート
印刷プレビュー

反応式

HRID 446028 の反応式
[Br:1][CH2:2][C:3]1[C:8]([Cl:9])=[CH:7][CH:6]=[CH:5][C:4]=1[CH2:10][OH:11]>[O-2].[O-2].[Mn+4].ClCCl>[Br:1][CH2:2][C:3]1[C:8]([Cl:9])=[CH:7][CH:6]=[CH:5][C:4]=1[CH:10]=[O:11]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 1

HCID 22121430[2-(Bromomethyl)-3-chlorophenyl]methanol

生成物 1

HCID 866782482-(Bromomethyl)-3-chlorobenzaldehyde収率 66.2%

試薬・触媒・溶媒 2

HCID 178418406HCID 178418406、化合物触媒2 回HCID 6344Dichloromethane溶媒

実験手順

Dichloromethane (15 ml) and manganese dioxide (1.69 g, 19.4 mmol) were added to [2-(bromomethyl)-3-chlorophenyl]methanol obtained in Example 10d (440 mg, 1.87 mmol), followed by stirring at mom temperature overnight. Manganese dioxide (1.2 g, 13.8 mmol) was further added, followed by heating with stirring at 40° C. for 2.5 hours. The reaction mixture was filtered through Celite and washed with ethyl acetate. The filtrate was concentrated under reduced pressure, and the resulting crude product was purified by column chromatography (silica gel, elution solvent: heptane/ethyl acetate=99/1->90/10) to give the title compound (289 mg, yield 66.2%).

このページの内容参加物実験手順後処理出典と根拠反応ノート

後処理

  1. temperatureby heating
  2. stirringwith stirring at 40° C. for 2.5 hours
  3. filtrationThe reaction mixture was filtered through Celite
  4. washwashed with ethyl acetate
  5. concentrationThe filtrate was concentrated under reduced pressure
  6. customthe resulting crude product was purified by column chromatography (silica gel, elution solvent: heptane/ethyl acetate=99/1->90/10)

出典と根拠

ORDレコード
ord-5232bbafd6294d8ca966fae313deae3c
出典データセット
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08476301B2

反応ノート

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