反応 #64673

反応方程式

1-Chloro-4-hydroxythioxanthone

potassium carbonate

n-Propyl bromide

→

title compound

収率 75.5%

1-Chloro-4-n-propoxythioxanthone

収率 75.5%

溶媒

acetone

反応条件

後処理

1. 1
   温度the resulting mixture heated
2. 2
   温度under reflux for 16 hours
3. 3
   温度The mixture was then cooled
4. 4
   その他quenched on to water (250 ml)
5. 5
   ろ過The solid was filtered
6. 6
   洗浄washed with water the resulting damp solid
7. 7
   その他recrystallised from ethanol (50 ml)

実験手順

1-Chloro-4-hydroxythioxanthone (7.8 g; 0.03 mol) prepared as above and potassium carbonate (5.0 g; 0.036 mol) was stirred and refluxed for 10 minutes in acetone (50 ml). n-Propyl bromide (5.5 g; 0.045 mol) was added and the resulting mixture heated under reflux for 16 hours. The mixture was then cooled and quenched on to water (250 ml). The solid was filtered and washed with water the resulting damp solid recrystallised from ethanol (50 ml) to afford the title compound (6.9 g; 75.5%) of mp 102°-3°. Analysis C16H13ClO2S=304.777 Requires C 63.05%; H 4.30%; Cl 11.63%; S 10.52% Found C 63.14%; H 4.37%; Cl 11.66%; S 10.63%

出典