반응 #55872

반응 방정식

water

potassium hydroxide

lithium chloride

α-trichloromethyl-2-thiophenemethanol

water

→

2-thiopheneglycolic acid

용매

diethylether

dioxane

반응 조건

후처리

1. 1
   workup.WAITat room temperature and for 3 hr
2. 2
   기타at 80° C
3. 3
   기타The ether soluble part was separated
4. 4
   추출extracted with diethylether
5. 5
   건조The organic layer was dried with anhydrous magnesium sulfate
6. 6
   workup.ADDITIONwas treated with activated carbon
7. 7
   여과filtered
8. 8
   농축Thereafter, the filtrate was concentrated

실험 절차

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.

출처