Реакция #9862

Уравнение реакции

2,5-Dihydroxy-1,4-dithiane

cyanoacetamide

methanol

→

title compound

Выход 141.7%

2-Amino-thiophene-3-carboxlic acid amide

Выход 141.7%

Растворители

triethylamine

water

water

Условия реакции

Обработка

1. 1
   ТемператураThe resulting mixture was heated at 35–40° C. for about 30 minutes
2. 2
   Температураheated to 50–60° C. for an additional 30 minutes
3. 3
   workup.STIRRINGwith stirring
4. 4
   ДругоеA fine precipitate formed upon addition, which
5. 5
   Фильтрацияwas filtered
6. 6
   Другоеdried overnight

Методика

2,5-Dihydroxy-1,4-dithiane (76 g) and cyanoacetamide (84 g) were added to a mixture of methanol (180 mL), water (10 mL) and triethylamine (10 g). The resulting mixture was heated at 35–40° C. for about 30 minutes while stirring, and then heated to 50–60° C. for an additional 30 minutes with stirring. The reaction mixture was then cooled to room temperature and poured into a mixture of ice (100 g)/water (300 mL). A fine precipitate formed upon addition, which was filtered and dried overnight to give 100.6 g of the title compound as a pale gray powder ((M+H)+=143, M.P.=159.0–159.6° C.).

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