Reaktion #2289929

Reaktionsgleichung

compound 11-3

ethyl trans-4-(4-((2-(2-amino-6-chlorophenyl)-2-oxoethyl)(3,5-difluorobenzyl)carbamoyl)-5-(trifluoromethyl)-1H-pyrazol-1-yl)cyclohexanecarboxylate

pyridine

CH3COCl

→

compound 13-1

Ausbeute 106.8%

ethyl trans-4-(4-((2-(2-acetamido-6-chlorophenyl)-2-oxoethyl)(3,5-difluorobenzyl)carbamoyl)-5-(trifluoromethyl)-1H-pyrazol-1-yl)cyclohexanecarboxylate

Ausbeute 106.8%

Lösungsmittel

DCM

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe reaction mixture was quenched with water (20 mL)
2. 2
   Extraktionextracted with DCM (2×10 mL)
3. 3
   WaschenThe combined organic layers were washed with water (50 mL), brine (50 mL)
4. 4
   Trocknendried over Na2SO4
5. 5
   Einengenconcentrated under reduced pressure
6. 6
   SonstigeThe residue was purified by column chromatography (silica gel, 20% EtOAc/hexane as eluent)

Vorschrift

To a stirred solution of compound 11-3 (45 mg, 0.07 mmol) in 1:1 mixture of pyridine and DCM (5 mL) was added CH3COCl (6 μL, 0.08 mmol) at 0° C. and stirred for 2 h. The reaction mixture was quenched with water (20 mL) and extracted with DCM (2×10 mL). The combined organic layers were washed with water (50 mL), brine (50 mL), dried over Na2SO4 and concentrated under reduced pressure. The residue was purified by column chromatography (silica gel, 20% EtOAc/hexane as eluent) to provide compound 13-1 (50 mg, quant.) as a yellow solid.

Quelle