Reaktion #56780

Reaktionsgleichung

compound 4c

3-[2(R)-tert-butoxycarbonylamino-2-cyclohexylethyl]-5-(2-fluoro-3-methoxyphenyl)-1-[2,6-difluorobenzyl]-6-methyl-pyrimidine-2,4(1H,3H)-dione

TFA

→

compound 4d

3-[2(R)-amino-2-cyclohexylethyl]-5-(2-fluoro-3-methoxyphenyl)-1-[2,6-difluorobenzyl]-6-methyl-pyrimidine-2,4(1H,3H)-dione

Lösungsmittel

dichloromethane

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeVolatiles were evaporated
2. 2
   Sonstigethe residue was partitioned between saturated NaHCO3/water and EtOAc
3. 3
   TrocknenThe organic layer was dried (sodium sulfate)
4. 4
   Sonstigeevaporated
5. 5
   Sonstigepurified by reverse phase HPLC(C-18 column, 15-75% ACN/water)

Vorschrift

To compound 4c (300 mg, 0.5 mmol) in dichloromethane (2 mL) was added TFA (2 mL) and the reaction mixture was stirred at ambient temperature for 1 hour. Volatiles were evaporated and the residue was partitioned between saturated NaHCO3/water and EtOAc. The organic layer was dried (sodium sulfate), evaporated, purified by reverse phase HPLC(C-18 column, 15-75% ACN/water) to give compound 4d . MS (CI) m/z 502.2 (MH+).

Quelle