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温度

0 °C

A 250 mL round bottom flask was charged with 2-(4-nitrophenyl)ethanimidamide hydrochloride (approximately 6.47 g, 30.0 mmol, 48% purity), triethyl ethane-1,1,2-tricarboxylate (7.60 mL, 33.0 mmol) and methanol (43 mL). To this solution was added a 25% sodium methoxide solution in methanol (24.0 mL, 105.2 mmol) immediately resulting in a dark purple thick suspension. After stirring for three hours under reflux the dark purple mixture was cooled to 0° C. using an ice bath and carefully treated with 30 mL water. This mixture was slowly treated with 35 mL 6N hydrochloric acid giving a pale green suspension. The suspension was stirred for additional 30 minutes, filtered and the obtained fawn solid was washed with 100 mL water. The product was dried in a desiccator under vacuum for two days. The crude product was used without purification in the next step.

1. customimmediately resulting in a dark purple thick suspension
2. temperatureunder reflux the dark purple mixture
3. stirringThe suspension was stirred for additional 30 minutes
4. filtrationfiltered
5. washthe obtained fawn solid was washed with 100 mL water
6. customThe product was dried in a desiccator under vacuum for two days
7. customThe crude product was used without purification in the next step