Bromine → 2-bromo-4H,5H,6H,7H-thieno(2,3-c)pyridine hydrobromide
反応式
[Br:1]Br.Cl.[S:4]1[C:8]2[CH2:9][NH:10][CH2:11][CH2:12][C:7]=2[CH:6]=[CH:5]1>C(O)(=O)C>[BrH:1].[Br:1][C:5]1[S:4][C:8]2[CH2:9][NH:10][CH2:11][CH2:12][C:7]=2[CH:6]=1参加物
4
実験手順
A solution of bromine (139 mg, 0.87 mmol) in acetic acid (0.5 mL) was added to a solution of 4,5,6,7-tetrahydrothieno[2,3-c]pyridine hydrochloride (150 mg, 0.85 mmol) in acetic acid (3 mL) and the mixture left to stir at ambient temperature for 1.5 h. The resultant precipitate was collected by filtration, washed with diethyl ether and left to air dry to afford the title compound as an off-white solid (230 mg, 90%). NMR (DMSO-D6, 300 MHz): 9.19 (s, 2H), 7.09 (s, 1H), 4.29-4.26 (m, 2H), 2.86-2.78 (m, 2H), 2.52-2.48 (m, 2H). LCMS (Method B): RT=1.65 min, M+H+=218/220.
後処理
- waitthe mixture left
- filtrationThe resultant precipitate was collected by filtration
- washwashed with diethyl ether
- waitleft to air
- customdry
出典と根拠
- ORDレコード
- ord-4a407b8b3ecf45a5bfea946ececea87b
- 出典データセット
- uspto-grants-2015_12
- 特許番号
- US09216980B2
反応ノート
読み込み中…