Reaktion #971706

Reaktionsgleichung

5-trifluoromethyl-pyridin-3-ylamine

pyridine

phenyl chloroformate

→

title compound

(5-Trifluoromethyl-pyridin-3-yl)-carbamic acid phenyl ester

Lösungsmittel

THF

DCM

Reaktionsbedingungen

Aufarbeitung

1. 1
   Waschenwashed with water (50 mL)
2. 2
   SonstigeThe organic layer is separated
3. 3
   Trocknendried over anhydrous Na2SO4
4. 4
   Filtrationfiltered
5. 5
   Einengenconcentrated
6. 6
   SonstigeThe residue is then separated via FCC (EtOAc/heptanes 1:9 to EtOAc/heptanes 1:1)

Vorschrift

Example 7-A, 5-trifluoromethyl-pyridin-3-ylamine, (385 mg, 2.37 mmol) is taken up in THF (25 mL) and pyridine (0.38 mL, 4.75 mmol) at 0° C. before phenyl chloroformate (558 mg, 3.56 mmol) is added. After 2 h, the reaction is diluted with DCM (50 mL) and washed with water (50 mL). The organic layer is separated, dried over anhydrous Na2SO4, filtered and concentrated. The residue is then separated via FCC (EtOAc/heptanes 1:9 to EtOAc/heptanes 1:1) to give the title compound. MS (ESI) m/z 283.0 (M+1).

Quelle