Boron tribromide → 5-Formyl-2,3-dihydroxybenzonitrile
반응식
[CH:1]([C:3]1[CH:4]=[C:5]([C:8]([OH:13])=[C:9]([O:11]C)[CH:10]=1)[C:6]#[N:7])=[O:2].B(Br)(Br)Br>ClCCl>[CH:1]([C:3]1[CH:4]=[C:5]([C:8]([OH:13])=[C:9]([OH:11])[CH:10]=1)[C:6]#[N:7])=[O:2]참가 물질
4
반응 조건
- 온도
- 0 °C
실험 절차
18 g of the product of Step A and 400 ml of dichloromethane were mixed together under nitrogen and the mixture was cooled to 0° C. 150 ml of a molar solution of boron tribromide in dichloromethane were added and the mixture stood for one night at ambient temperature. It was concentrated, cooled again to 0° C. and 250 ml of a normal solution of hydrochloric acid were added. The crystallized product was separated out, washed with water, dried then crystallized from an isopropanol--water mixture (1-2) to obtain 12 g of the expected product.
후처리
- waitthe mixture stood for one night at ambient temperature
- concentrationIt was concentrated
- temperaturecooled again to 0° C.
- addition250 ml of a normal solution of hydrochloric acid were added
- customThe crystallized product was separated out
- washwashed with water
- customdried
- customthen crystallized from an isopropanol
출처 및 근거
- ORD 기록
- ord-8ff9fcd9cfe74e8dbd93a16959bf292e
- 출처 데이터셋
- uspto-grants-1998_03
- 특허 번호
- US05728828
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