反応 #726972

反応方程式

Methyl iodide

1,3-diazepane-2-thione

EtOH

→

crude title compound

収率 86.0%

2-(methylthio)-4,5,6,7-tetrahydro-1H-1,3-diazepine

収率 86.0%

溶媒

acetone

反応条件

後処理

1. 1
   温度The reaction mixture was refluxed for 15 min
2. 2
   workup.DISSOLUTIONto dissolve the solids
3. 3
   workup.ADDITIONwas added
4. 4
   ろ過the precipitate was collected by filtration
5. 5
   洗浄washed with hex
6. 6
   その他and dried

実験手順

Methyl iodide (0.55 ml, 1.15 mmol) was added to a solution of 1,3-diazepane-2-thione (1.00 g, 7.68 mmol) in acetone (8 ml). The reaction mixture was refluxed for 15 min. EtOH was added to the hot solution to dissolve the solids. After cooling to r.t. hex. was added and the precipitate was collected by filtration, washed with hex. and dried to give 1.79 g (86%) crude title compound which was used directly in the next step.

出典