反应详情

温度

-4 °C

Nicotinic acid (2.14 g, 0.017 mol) was suspended in 75 mL of dry tetrahydrofuran, then 1.76 g of freshly distilled triethylamine were added. The clear solution thus obtained was cooled to -4° C. in an ice bath under argon, then ethyl chloroformate (1.88 g, 0.014 mol) in 10 mL of tetrahydrofuran was added such that the temperature did not go above 0° C. The free aminocyclohexanol (2.0 g, 0.017 mol) was added as a powder to the cold reaction mixture, which was allowed to come to room temperature and stirred for 2 hours. The precipitate which formed was collected by filtration, dissolved in 28 mL of hot water and recrystallized as 3.25 g (85%) of fine colorless needles melting at 208°-210° C. and having the formula ##STR113## as confirmed by elemental analysis.

1. customThe clear solution thus obtained
2. customdid not go above 0° C
3. customto come to room temperature
4. customThe precipitate which formed
5. filtrationwas collected by filtration
6. dissolutiondissolved in 28 mL of hot water
7. customrecrystallized as 3.25 g (85%) of fine colorless needles melting at 208°-210° C.