Formamide → N-Formylleucine

Temperature

100 °C

165.2 g of L-leucine and 821.7 g of formamide are introduced, under a nitrogen atmosphere, into a reactor equipped with a stirrer system. The mixture is heated at 100° C. for approximately 6 hours. Approximately 513 g of formamide are then removed by distillation under a pressure of 20 -30 mm of mercury and at a pot temperature of 50°-60° C. 1082 g of water are subsequently added to the mixture. It is cooled to 20°-25° C. It is then acidified to pH 2.5 with sulphuric acid. It is stirred for 2 hours at approximately 20° C. and then for one hour at 5° C. Filtration is carried out and the cake is rinsed with 100 g of water at pH 2. It is dried under vacuum. 180.3 g of N-formyl-L-leucine are thus obtained (90% yield) with an optical rotation [α]D20=−17.7° (c=1 in ethanol), i.e. a purity of 98.3%.

1. customequipped with a stirrer system
2. customApproximately 513 g of formamide are then removed by distillation under a pressure of 20 -30 mm of mercury and at a pot temperature of 50°-60° C
3. addition1082 g of water are subsequently added to the mixture
4. temperatureIt is cooled to 20°-25° C
5. waitfor one hour at 5° C
6. filtrationFiltration
7. washthe cake is rinsed with 100 g of water at pH 2
8. customIt is dried under vacuum

ORD record

ord-2f30c4a0603f48698652dfc908f0fc2c

Source dataset

uspto-grants-2001_09

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06294692B1