Bromine → HCID 57466726、化合物
反応式
[CH3:1][CH:2]1[N:7]([CH3:8])[CH2:6][C:5]2[S:9][CH:10]=[CH:11][C:4]=2[CH2:3]1.FC(F)(F)C([O-])=O.[Br-:19].[K+].BrBr>O>[Br:19][C:10]1[S:9][C:5]2[CH2:6][N:7]([CH3:8])[CH:2]([CH3:1])[CH2:3][C:4]=2[CH:11]=1参加物
6
実験手順
1.0 g (3.6 mmol) 5,6-dimethyl-4,5,6,7-tetrahydro-thieno[2,3-c]pyridine (as the trifluoroacetate salt) are dissolved in 60 ml of water and at the temperature of an ice bath combined with a solution of 1.0 g (8.5 mmol) potassium bromide and 182 μl (3.6 mmol) bromine in 20 ml of water. The mixture is stirred for 2.5 hours in the ice bath and then extracted twice with 100 ml ethyl acetate. The combined organic phases are washed with sat. sodium chloride solution, then dried on sodium sulphate and evaporated down i. vac. The crude product thus obtained is purified by chromatography on silica gel (eluant DCM/methanol 50:1).
後処理
- extractionextracted twice with 100 ml ethyl acetate
- washThe combined organic phases are washed with sat. sodium chloride solution
- customdried on sodium sulphate
- customevaporated down i
出典と根拠
- ORDレコード
- ord-022e953da41749cfa28ff4b5d96536dc
- 出典データセット
- uspto-grants-2012_11
- 特許番号
- US08309542B2
反応ノート
読み込み中…