反应 #55872

反应方程式

water

potassium hydroxide

lithium chloride

α-trichloromethyl-2-thiophenemethanol

water

→

2-thiopheneglycolic acid

溶剂

diethylether

dioxane

反应条件

后处理

1. 1
   workup.WAITat room temperature and for 3 hr
2. 2
   其他at 80° C
3. 3
   其他The ether soluble part was separated
4. 4
   萃取extracted with diethylether
5. 5
   干燥The organic layer was dried with anhydrous magnesium sulfate
6. 6
   workup.ADDITIONwas treated with activated carbon
7. 7
   过滤filtered
8. 8
   浓缩Thereafter, the filtrate was concentrated

实验过程

Into 2.4 ml of water, potassium hydroxide (0.67 g, 12 mmol) and lithium chloride (0.254 g, 6 mmol) were dissolved. Then, into the solution above, α-trichloromethyl-2-thiophenemethanol (0.693 g, 3 mmol) solution in dioxane (2.4 ml) was added and agitation was conducted for 12 hr. at room temperature and for 3 hr. at 80° C. Thereafter, water (20 ml) was added thereto and diethylether was further added into the reaction mixture. The ether soluble part was separated. The water layer was acidified with hydrochloric acid and then, extracted with diethylether. The organic layer was dried with anhydrous magnesium sulfate and was treated with activated carbon and filtered. Thereafter, the filtrate was concentrated and gave 0.246 g of 2-thiopheneglycolic acid as crystals.

来源