2-Hydroxy-3,4,6-trimethylbenzaldehyde → 2,3,5,6-Tetramethylphenol

HRID 453419

反応式

HRID 453419 の反応式
[OH:1][C:2]1[C:9]([CH3:10])=[C:8]([CH3:11])[CH:7]=[C:6]([CH3:12])[C:3]=1[CH:4]=O>CO.[C].[Pd]>[CH3:4][C:3]1[C:6]([CH3:12])=[CH:7][C:8]([CH3:11])=[C:9]([CH3:10])[C:2]=1[OH:1]

参加物

4

反応物 1

HCID 113211462-Hydroxy-3,4,6-trimethylbenzaldehyde

生成物 1

HCID 106942,3,5,6-Tetramethylphenol収率 12.1%

試薬・触媒・溶媒 2

HCID 178418390HCID 178418390、化合物触媒HCID 887Methanol溶媒

実験手順

2-Hydroxy-3,4,6-trimethylbenzaldehyde (6.58 g, 40.1 mmol) was dissolved in methanol (120 mL), 10% palladium-carbon (50% water-containing product, 1.0 g) was added under hydrogen atmosphere (balloon pressure), and the mixture was stirred at room temperature for 22 hr. The catalyst was filtered off, and the filtrate was concentrated under reduced pressure. The precipitated crystals were recrystallized from methanol to give the title compound (0.73 g, yield 12%) as colorless crystals. The mother solution was concentrated under reduced pressure to give second crop (5.10 g, yield 85%).

後処理

  1. filtrationThe catalyst was filtered off
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. customThe precipitated crystals were recrystallized from methanol

出典と根拠

ORDレコード
ord-dc76604064ae4a79a08bba08857ce0dc
出典データセット
uspto-grants-2013_07
特許番号
US08492430B2

関連ノート

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