Sodium methanethiolate → 4-Methyl-5-(methylsulfanyl)-1,3-thiazol-2-amine
反応式
Br[C:2]1[S:6][C:5]([NH2:7])=[N:4][C:3]=1[CH3:8].[CH3:9][S-:10].[Na+]>CO>[CH3:8][C:3]1[N:4]=[C:5]([NH2:7])[S:6][C:2]=1[S:10][CH3:9]参加物
4
実験手順
5-Bromo-4-methyl-thiazol-2-ylamine (1.35 g, 7 mmol,) was dissolved in methanol abs. (13.5mL) and sodium methanethiolate (0.6 g, 7.7 mmol) 1.1 equiv.) was added portionwise at rt. After stirring overnight, the dark colored mixture was concentrated under reduced pressure and purified over a 50 g silica cartridge (NH2-modified) with ethyl acetate as eluent. The desired fractions were evaporated to give the title compound as a light yellow solid: 180 mg, MS (ISP): m/e 161.1 (M+H)+
後処理
- concentrationthe dark colored mixture was concentrated under reduced pressure
- custompurified over a 50 g silica cartridge (NH2-modified) with ethyl acetate as eluent
- customThe desired fractions were evaporated
出典と根拠
- ORDレコード
- ord-99a3bb1bee3d470295e3d3edce32c9b4
- 出典データセット
- uspto-grants-2011_07
- 特許番号
- US07973051B2
反応ノート
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