Bromine → 3-Bromo-5,6,7,9-tetrahydro-pyrido[2,3-b]azepin-8-one
반응식
[Br:1]Br.[N:3]1[C:8]2[NH:9][C:10](=[O:14])[CH2:11][CH2:12][CH2:13][C:7]=2[CH:6]=[CH:5][CH:4]=1>C(Cl)Cl>[Br:1][C:5]1[CH:4]=[N:3][C:8]2[NH:9][C:10](=[O:14])[CH2:11][CH2:12][CH2:13][C:7]=2[CH:6]=1참가 물질
4
실험 절차
A 10% solution of bromine (0.57 mL, 11.1 mmole) in CH2Cl2 was added dropwise over 1 hr to a solution of 5,6,7,9-tetrahydro-pyrido[2,3-b]azepin-8-one (1.20 g, 7.4 mmole) in CH2Cl2 at RT. The mixture was stirred at RT overnight, then was concentrated in vacuo. The residue was diluted with 10% Na2CO3 and extracted with EtOAc. The combined organics were dried over Na2SO4 and concentrated. Flash chromatography on silica gel (EtOAc) gave the title compound (1.00 g, 56%) as a light yellow solid after drying in vacuo: MS (ES) m/e 241/243.
후처리
- concentrationwas concentrated in vacuo
- additionThe residue was diluted with 10% Na2CO3
- extractionextracted with EtOAc
- dry with materialThe combined organics were dried over Na2SO4
- concentrationconcentrated
출처 및 근거
- ORD 기록
- ord-df55d09ad9de476086716ba789c1081d
- 출처 데이터셋
- uspto-grants-2011_02
- 특허 번호
- US07879872B2
반응 노트
불러오는 중…