تفاعل #55872

ord-c8f460d8f5214d67a7ca573726d7dc2c

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.WAITat room temperature and for 3 hr
  2. 2
    أخرىat 80° C
  3. 3
    أخرىThe ether soluble part was separated
  4. 4
    استخلاصextracted with diethylether
  5. 5
    تجفيفThe organic layer was dried with anhydrous magnesium sulfate
  6. 6
    workup.ADDITIONwas treated with activated carbon
  7. 7
    ترشيحfiltered
  8. 8
    تركيزThereafter, the filtrate was concentrated

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04221915uspto-grants-1980_09