2-Methyl-5-nitrobenzoic acid → (2-Methyl-5-nitrophenyl)methanol

HRID 1946343

反応式

HRID 1946343 の反応式
[CH3:1][C:2]1[CH:10]=[CH:9][C:8]([N+:11]([O-:13])=[O:12])=[CH:7][C:3]=1[C:4](O)=[O:5]>C1COCC1.CO>[CH3:1][C:2]1[CH:10]=[CH:9][C:8]([N+:11]([O-:13])=[O:12])=[CH:7][C:3]=1[CH2:4][OH:5]

参加物

4

反応物 1

HCID 5196832-Methyl-5-nitrobenzoic acid

生成物 1

HCID 3567085(2-Methyl-5-nitrophenyl)methanol収率 114.6%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒2 回HCID 8028Tetrahydrofuran溶媒

反応条件

温度
80 °C

実験手順

To a solution of 2-methyl-5-nitrobenzoic acid (3.0 g, 16.6 mmol, Acros) in THF (60 ml) at ambient temperature under nitrogen was added dropwise 1.0 M borane-tetrahydrofuran complex (33.1 ml, 33.1 mmol, Aldrich). The solution was heated to 80° C. for 1.5 h. To the solution at ambient temperature was slowly added methanol (20 ml) and then heated to 80° C. for 30 min. The solvent was removed in vacuo to leave an oil. The residue was dissolved in methanol (approximately 30 ml) and the solvent removed in vacuo to give (2-methyl-5-nitrophenyl)methanol as a yellow solid (3.18 g).

後処理

  1. customat ambient temperature
  2. temperatureheated to 80° C. for 30 min
  3. customThe solvent was removed in vacuo
  4. customto leave an oil
  5. customthe solvent removed in vacuo

出典と根拠

ORDレコード
ord-a27c82ea6a4045009aa1b2b79a3bb9cd
出典データセット
uspto-grants-2013_03
特許番号
US08399436B2

関連ノート

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