تفاعل #971706

معادلة التفاعل

5-trifluoromethyl-pyridin-3-ylamine

pyridine

phenyl chloroformate

→

title compound

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

المذيبات

THF

DCM

ظروف التفاعل

المعالجة

1. 1
   غسيلwashed with water (50 mL)
2. 2
   أخرىThe organic layer is separated
3. 3
   تجفيفdried over anhydrous Na2SO4
4. 4
   ترشيحfiltered
5. 5
   تركيزconcentrated
6. 6
   أخرىThe residue is then separated via FCC (EtOAc/heptanes 1:9 to EtOAc/heptanes 1:1)

الإجراء التجريبي

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).

المصدر