Cyclopentylamine → 5-bromo-N-cyclopentyl-2-nitroaniline
반응식
[CH:1]1([NH2:6])[CH2:5][CH2:4][CH2:3][CH2:2]1.Br[C:8]1[CH:13]=[C:12]([Br:14])[CH:11]=[CH:10][C:9]=1[N+:15]([O-:17])=[O:16]>C(O)CCC>[Br:14][C:12]1[CH:11]=[CH:10][C:9]([N+:15]([O-:17])=[O:16])=[C:8]([NH:6][CH:1]2[CH2:5][CH2:4][CH2:3][CH2:2]2)[CH:13]=1참가 물질
4
반응 조건
- 온도
- 100 °C
실험 절차
Add cyclopentanamine (32 mL) to a solution of 2,4-dibromo-1-nitro-benzene (20 g) in 1-butanol (160 mL). Heat the mixture at 100° C. overnight. Remove the solvent under vacuum, add water and extract with EA. Wash the organic layer sequentially with an aqueous saturated solution of sodium bicarbonate and then water. Dry over magnesium sulfate and remove the solvent under vacuum to afford 22 g of the title compound. MS (ES+): m/z=286 (M+H)+.
후처리
- customRemove the solvent under vacuum
- additionadd water
- extractionextract with EA
- washWash the organic layer sequentially with an aqueous saturated solution of sodium bicarbonate
- dry with materialDry over magnesium sulfate
- customremove the solvent under vacuum
출처 및 근거
- ORD 기록
- ord-a3fe5ae5977840999ea2a400945b6900
- 출처 데이터셋
- uspto-grants-2010_12
- 특허 번호
- US07855211B2
반응 노트
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