Boron tribromide → 3-Chloro-4,5-dihydroxybenzaldehyde
반응식
[Cl:1][C:2]1[C:3]([OH:12])=[C:4]([O:10]C)[CH:5]=[C:6]([CH:9]=1)[CH:7]=[O:8].B(Br)(Br)Br>ClCCl>[Cl:1][C:2]1[CH:9]=[C:6]([CH:5]=[C:4]([OH:10])[C:3]=1[OH:12])[CH:7]=[O:8]참가 물질
4
반응 조건
- 온도
- 0 °C
실험 절차
37.2 g of commercial 5-chloro vanillin and 800 ml of dichloromethane were mixed together under nitrogen and cooled to 0° C. 300 ml of a molar solution of boron tribromide in dichloromethane are added and the mixture stood for one night at ambient temperature. It was concentrated, cooled again to 0° C. and acidified. The crystallized product was separated, washed with water, dried and crystallized from an isopropanol- water mixture (1-2 by volume) to obtain 26.6 g of the expected product melting at >260° C.
후처리
- waitthe mixture stood for one night at ambient temperature
- concentrationIt was concentrated
- temperaturecooled again to 0° C.
- customThe crystallized product was separated
- washwashed with water
- customdried
- customcrystallized from an isopropanol- water mixture (1-2 by volume)
출처 및 근거
- ORD 기록
- ord-49d72313e0d6412c95d675c45339c241
- 출처 데이터셋
- uspto-grants-1998_03
- 특허 번호
- US05728828
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