Homovanillyl alcohol → 4-Hydroxy-3-methoxyphenethyl chloride
반응식
S(Cl)([Cl:3])=O.[OH:5][C:6]1[CH:14]=[CH:13][C:9]([CH2:10][CH2:11]O)=[CH:8][C:7]=1[O:15][CH3:16]>ClCCl>[OH:5][C:6]1[CH:14]=[CH:13][C:9]([CH2:10][CH2:11][Cl:3])=[CH:8][C:7]=1[O:15][CH3:16]참가 물질
4
실험 절차
Thionyl chloride (0.5 ml) was added, dropwise, to a! stirred solution of 4-hydroxy-3-methoxyphenethyl alcohol (0.83 g--commercially available) in dichloromethane (50 ml). When the addition was complete, the mixture was heated under reflux for 3 hours. On cooling to room temperature, the mixture was concentrated in vacuo to give a gum which was purified by column chromatography on silica eluting with dichloromethane containing methanol (0% up to 2%). The product-containing fractions were combined and concentrated in vacuo to give the title compound as an oil, yield 0.36 g.
후처리
- additionWhen the addition
- temperaturethe mixture was heated
- temperatureunder reflux for 3 hours
- concentrationthe mixture was concentrated in vacuo
- customto give a gum which
- customwas purified by column chromatography on silica eluting with dichloromethane
- additioncontaining methanol (0% up to 2%)
- concentrationconcentrated in vacuo
출처 및 근거
- ORD 기록
- ord-124c450056884168846253c87de29ffb
- 출처 데이터셋
- uspto-grants-1995_06
- 특허 번호
- US05422358
반응 노트
불러오는 중…