反応 #55872

反応方程式

water

potassium hydroxide

lithium chloride

α-trichloromethyl-2-thiophenemethanol

water

→

2-thiopheneglycolic acid

溶媒

diethylether

dioxane

反応条件

後処理

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

実験手順

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.

出典