Dichloromethane → N-(2-aminoethyl)-3-bromopyridine-2-carboxamide hydrochloride
반응식
[Br:1][C:2]1[C:3]([C:8]([NH:10][CH2:11][CH2:12][NH:13]C(=O)OC(C)(C)C)=[O:9])=[N:4][CH:5]=[CH:6][CH:7]=1.FC(F)(F)C(O)=O.C(Cl)[Cl:29]>>[ClH:29].[NH2:13][CH2:12][CH2:11][NH:10][C:8]([C:3]1[C:2]([Br:1])=[CH:7][CH:6]=[CH:5][N:4]=1)=[O:9]참가 물질
4
실험 절차
3.2 g of t-butyl [2-(3-bromopyridine-2-carboxamido)ethyl]carbamate were heated to reflux for 4 hours with 3.5 ml of methylene chloride and 3.5 ml of trifluoroacetic acid. The reaction mixture was concentrated under reduced pressure, the residue was dissolved in ethanol and the solution was treated with an equimolar amount of ethanolic hydrochloric acid. The hydrochloride was recrystallized from methanol/ether, whereby there was obtained N-(2-aminoethyl)-3-bromopyridine-2-carboxamide hydrochloride as white crystals, m.p. 279°.
후처리
- concentrationThe reaction mixture was concentrated under reduced pressure
- dissolutionthe residue was dissolved in ethanol
- additionthe solution was treated with an equimolar amount of ethanolic hydrochloric acid
- customThe hydrochloride was recrystallized from methanol/ether
출처 및 근거
- ORD 기록
- ord-041fa8d9cec1462ca5db313f84321533
- 출처 데이터셋
- uspto-grants-1988_08
- 특허 번호
- US04764522
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