Reaktion #162761

Reaktionsgleichung

Intermediate 6b

4-Amino-1-p-tolyl-1H-pyrazole

triethylamine

trichloroethyl chloroformate

→

title compound

Ausbeute 95.0%

(1-p-Tolyl-1H-pyrazol-4-yl)-carbamic acid 2,2,2-trichloro-ethyl ester

Ausbeute 95.0%

Lösungsmittel

DCM

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturwas cooled
2. 2
   Temperaturwith cooling for 45 min
3. 3
   Sonstigeevaporated to dryness
4. 4
   SonstigeResidue was purified by FCC
5. 5
   Wascheneluting with 0-30% ethyl acetate in cyclohexane

Vorschrift

Intermediate 6b (150 mg, 0.87 mmol) dissolved in DCM (10 mL) was cooled using an ice bath, and then treated sequentially with triethylamine (0.18 mL, 1.30 mmol) and trichloroethyl chloroformate (0.15 mL, 1.08 mmol). The mixture was stirred with cooling for 45 min, then evaporated to dryness. Residue was purified by FCC, eluting with 0-30% ethyl acetate in cyclohexane, to give the title compound as a beige solid (286 mg, 95%). LCMS (Method 3): Rt 4.25 min, m/z 348/350/352 [MH+].

Quelle