反応 #8941

反応方程式

2-carbomethoxyamino-benzimidazole

chlorosulfonic acid

→

desired compound

収率 78.0%

5-Chlorosulfonyl-2-carbomethoxyamino-benzimidazole

収率 78.0%

反応条件

後処理

1. 1
   ろ過The resulting precipitate was filtered
2. 2
   洗浄washed throughly with cold water (500 ml)
3. 3
   乾燥The solid was dried overnight under high vacuum in a desiccator over NaOH pallets

実験手順

A solution of 2-carbomethoxyamino-benzimidazole (5.0 g, 0.026 mole) in chlorosulfonic acid (35.00 mL) was stirred at 0° C. for 30 min. and at room temperature for 3 hr. The resulting dark colored reaction mixture was carefully poured into an ice-water mixture (200 mL) and stirred at room temperature for 30 min. The resulting precipitate was filtered and washed throughly with cold water (500 ml). The solid was dried overnight under high vacuum in a desiccator over NaOH pallets to yield the desired compound (5.9 g. 78%) as a grey powder. 1H NMR (DMSO-d6) 3.89 (s, 3H), 7.55 (d, 1H, J=8.4 Hz.) 7.65 (d, 1H, J=8.4 Hz), 7.88 (s, 1H).

出典