Reacción #505187

Ecuación de reacción

2-Amino-5-methylpyrazine

pyridine

phenyl chloroformate

→

product

Rendimiento 68.7%

(5-Methylpyrazin-2-yl)carbamic acid phenyl ester

Rendimiento 68.7%

Disolventes

CH2Cl2

Condiciones de reacción

Tratamiento posterior

1. 1
   Otroto form
2. 2
   workup.STIRRINGThe mixture was stirred at 0° C. for 1 h
3. 3
   OtroThen the reaction was quenched with 0.25 M HCl (40 mL) and anhydrous ether (50 mL)
4. 4
   workup.STIRRINGstirred at 0° C., for 30 min
5. 5
   OtroThe precipitate was isolated by filtration
6. 6
   Lavadowashed with DI H2O (20 mL) and ether (2×25 mL)
7. 7
   Otrodried under vacuum

Procedimiento

2-Amino-5-methylpyrazine (5.16 g, 47 mmol) was dissolved in CH2Cl2 (52 mL), stirred and cooled to 0° C. under N2. To this, pyridine (4.8 mL, 59 mmol) was added followed by phenyl chloroformate (6.2 mL, 59 mmol), dropwise, over 15 min, causing a precipitate to form. The mixture was stirred at 0° C. for 1 h. Then the reaction was quenched with 0.25 M HCl (40 mL) and anhydrous ether (50 mL), and stirred at 0° C., for 30 min. The precipitate was isolated by filtration, washed with DI H2O (20 mL) and ether (2×25 mL), and dried under vacuum to give the product (7.4 g) as a white fluffy powder.

Fuente