반응식
[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]참가 물질
4
실험 절차
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%).
후처리
- filtrationThe catalyst was filtered off
- concentrationthe filtrate was concentrated under reduced pressure
- customThe precipitated crystals were recrystallized from methanol
출처 및 근거
- ORD 기록
- ord-6a6c79544d314ca99af80cbe738d22a3
- 출처 데이터셋
- uspto-grants-2012_01
- 특허 번호
- US08088821B2
연결된 노트
불러오는 중…