Diisopropylamine → 1-Bromo-3-chloro-2,4-difluorobenzene
반응식
C(NC(C)C)(C)C.C([Li])CCC.[F:13][C:14]1[CH:19]=[C:18]([F:20])[CH:17]=[CH:16][C:15]=1[Br:21].[Cl:22]C(Cl)(Cl)C(C(Cl)(Cl)Cl)=O>O1CCCC1>[Cl:22][C:19]1[C:14]([F:13])=[C:15]([Br:21])[CH:16]=[CH:17][C:18]=1[F:20]참가 물질
6
반응 조건
- 온도
- 0 °C
실험 절차
To a solution of 19 ml (0.135 mole) of diisopropylamine in 125 ml of tetrahydrofuran (THF) cooled at −20° C. is added 80 ml of n-butyllithium (1.6 M in hexane). The temperature is raised to 0° C. for 5 minutes and lowered to −78° C. Then 25 g (0.129 mole) of 2,4-difluoro-bromobenzene is then added and the reaction is stirred at 65° C. for 2 hours. Then, 25 ml (0.164 mole) of hexachloroacetone is added and the solution is warmed at room temperature. After evaporation of the solvent, the residue is distilled under vacuum to give the desired product.
후처리
- customlowered to −78° C
- temperaturethe solution is warmed at room temperature
- customAfter evaporation of the solvent
- distillationthe residue is distilled under vacuum
출처 및 근거
- ORD 기록
- ord-26d3f179119941d39512cec2ecd01884
- 출처 데이터셋
- uspto-grants-2005_02
- 특허 번호
- US06849740B2
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