Water → 5-(Bromomethyl)benzo[d]oxazole
반응식
[CH3:1][C:2]1[CH:3]=[CH:4][C:5]2[O:9][CH:8]=[N:7][C:6]=2[CH:10]=1.[Br:11]N1C(=O)CCC1=O.O>C(Cl)(Cl)Cl>[Br:11][CH2:1][C:2]1[CH:3]=[CH:4][C:5]2[O:9][CH:8]=[N:7][C:6]=2[CH:10]=1참가 물질
5
실험 절차
A solution of 5-methylbenzoxazole (0.5 g) in chloroform (20 ml) containing N-bromosuccinimide (0.18 g) and azoisobutyronitrile (0.05 g) was refluxed for 2 hours. After allowing to cool to room temperature the reaction mixture was treated with water (30 ml). The organic phase was separated and the aqueous phase extracted with dichloromethane (30 ml). The combined organic phases were washed with brine (30 ml), dried over magnesium sulphate and evaporated. The residue was triturated with pentane giving the title compound (0.36 g) as an off-white solid, m.p. 90-93° C.
후처리
- temperaturewas refluxed for 2 hours
- customThe organic phase was separated
- extractionthe aqueous phase extracted with dichloromethane (30 ml)
- washThe combined organic phases were washed with brine (30 ml)
- dry with materialdried over magnesium sulphate
- customevaporated
- customThe residue was triturated with pentane giving the title compound (0.36 g) as an off-white solid, m.p. 90-93° C.
출처 및 근거
- ORD 기록
- ord-42fa2a3da2d14b809218e78819ccab3c
- 출처 데이터셋
- uspto-grants-2000_04
- 특허 번호
- US06048893
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