Dichloromethane → N-(2-aminoethyl)-3-bromopyridine-2-carboxamide hydrochloride
反応式
[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]参加物
4
実験手順
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°.
後処理
- 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
出典と根拠
- ORDレコード
- ord-041fa8d9cec1462ca5db313f84321533
- 出典データセット
- uspto-grants-1988_08
- 特許番号
- US04764522
反応ノート
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