反応 #9862

反応方程式

2,5-Dihydroxy-1,4-dithiane

cyanoacetamide

methanol

→

title compound

収率 141.7%

2-Amino-thiophene-3-carboxlic acid amide

収率 141.7%

溶媒

triethylamine

water

water

反応条件

後処理

1. 1
   温度The resulting mixture was heated at 35–40° C. for about 30 minutes
2. 2
   温度heated to 50–60° C. for an additional 30 minutes
3. 3
   workup.STIRRINGwith stirring
4. 4
   その他A fine precipitate formed upon addition, which
5. 5
   ろ過was filtered
6. 6
   その他dried overnight

実験手順

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.).

出典