Bromochloromethane → 5-Chloromethylthio-1-methyltetrazole
反応式
O.[SH:2][C:3]1[N:7]([CH3:8])[N:6]=[N:5][N:4]=1.[Na].Br[CH2:11][Cl:12]>CC#N>[Cl:12][CH2:11][S:2][C:3]1[N:7]([CH3:8])[N:6]=[N:5][N:4]=1参加物
4
実験手順
A solution of sodium 5-mercapto-1-methyltetrazole hydrate (1.38 g, 10.0 mmol) in CH3CN (50 mL) was cooled in ice and treated in one portion with bromochloromethane (6.47 g, 50 mmol). The ice-bath was removed and the reaction mixture stirred at R.T. for 18 h. Then the solvent was evaporated and the crude product purified by chromatography on silica gel (eluted with CH2Cl2) to afford 1.27 g (77%) of the title compound, m.p.: 55°-57° C.
後処理
- customThe ice-bath was removed
- customThen the solvent was evaporated
- customthe crude product purified by chromatography on silica gel (eluted with CH2Cl2)
出典と根拠
- ORDレコード
- ord-fe4db918087f4216b4a060603599d86d
- 出典データセット
- uspto-grants-1992_05
- 特許番号
- US05116833
反応ノート
読み込み中…