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
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
- filtrationThe catalyst was filtered off
- concentrationthe filtrate was concentrated under reduced pressure
- customThe precipitated crystals were recrystallized from methanol
出典と根拠
- ORDレコード
- ord-c8ef37b0098c486e9cda2210405040db
- 出典データセット
- uspto-grants-2010_06
- 特許番号
- US07732626B2
関連ノート
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