1,2-Dichloroethane → 1-(3-Chloro-2-(2,2,2-trifluoroethoxy)phenylacetyl)-2-carbamoyl-4-(2-methylphenyl)piperazine

To a stirred solution of 2-(2,2,2-trifluoroethoxy)-3-chlorophenylacetic acid (0.14 g, 0.53 mmol) from Step 4 above, 2-carbamoyl-4-(2-methylphenyl)piperazine (0.12 g, 0.53 mmol) from Step 4 of Example 1, and HOBT (0.08 g, 0.53 mmol) in DMF (5 mL) was added EDC (0.15 g, 0.8 mmol) and DIEA (0.14 mL, 0.8 mmol). The mixture was stirred at ambient temperature for 14 h. The solvent was removed under reduced pressure and the residue was purified by preparative reverse phase HPLC using a H2O:CH3CN gradient containing 0.1% TFA. The product-containing fractions were lyophilized to give the title compound as an amorphous powder.

1. customThe solvent was removed under reduced pressure
2. customthe residue was purified by preparative reverse phase HPLC
3. additionCH3CN gradient containing 0.1% TFA

ORDレコード

ord-59047cab10664b81b97b07b9302d2f8f

出典データセット

uspto-grants-1999_10

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05968938