Reaktion #11348

Reaktionsgleichung

2-carbomethoxyamino-benzimidazole

chlorosulfonic acid

→

5-chlorosulfonyl-2-carbomethoxyamino-benzimidazole

Ausbeute 78.0%

Reaktionsbedingungen

Aufarbeitung

1. 1
   FiltrationThe resulting precipitate was filtered
2. 2
   Waschenwashed with cold water (500 mL)
3. 3
   TrocknenThe solid was dried overnight under high vacuum in a desiccator over NaOH pellets

Vorschrift

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 minutes and at room temperature for 3 hours. The resulting dark colored reaction mixture was poured into an ice-water mixture (200 mL), and stirred at room temperature for 30 minutes. The resulting precipitate was filtered and washed with cold water (500 mL). The solid was dried overnight under high vacuum in a desiccator over NaOH pellets to give 5-chlorosulfonyl-2-carbomethoxyamino-benzimidazole (5.9 g, 78%) as a grey powder. 1H NMR DMSO-d6) d: 3.89 (s, 3H), 7.55 (d, J=8.4 Hz, 1H), 7.65 (d, J=8.4 Hz, 1H), 7.88 (s, 1H). (German Patent DE 3826036)

Quelle