تفاعل #72640

معادلة التفاعل

2-amino-6-methylbenzonitrile

sulfamide

→

title compound

N-(2-Cyano-3-methylphenyl)sulfamide

المذيبات

1,4-dioxane

ظروف التفاعل

المعالجة

1. 1
   ترشيحthe precipitate was filtered
2. 2
   غسيلwashed with dioxane
3. 3
   تركيزThe filtrate was concentrated under reduced pressure
4. 4
   أخرىthe residue was purified by chromatography on silica gel eluting with EtOAc/hexanes (3:7)

الإجراء التجريبي

A solution of 2-amino-6-methylbenzonitrile (1.32 g, 10 mmol) and sulfamide (4.81 g, 50 mmol) in dry 1,4-dioxane (50 mL) was refluxed under nitrogen for 3 days. After the reaction mixture was cooled down to room temperature, the precipitate was filtered and washed with dioxane. The filtrate was concentrated under reduced pressure, and the residue was purified by chromatography on silica gel eluting with EtOAc/hexanes (3:7) to give the title compound as a pale-white solid. 1H NMR (400 MHz, DMSO-d6) δ2.44 (s, 3H), 7.19-7.21 (m, 3H), 7.39-7.41 (d, J=8.4 Hz, 1H), 7.53 (t, J=8.0 Hz, 1H), 9.41 (s, 1H).

المصدر