Triethylamine → Ethyl [2-methyl-4-({pentyl[4'-(trifluoromethyl)-1,1'-biphenyl-3-yl]amino}sulfonyl)phenoxy]acetate

To a solution of N-pentyl-N-[4′-(trifluoromethyl)-1,1′-biphenyl-3-yl]amine (70.6 mg, 0.23 mmol) in CH2Cl2 (5 mL) under nitrogen at room temperature was added ethyl [4-(chlorosulfonyl)-2-methylphenoxy]acetate (101 mg, 0.35 mmol) and triethylamine (96 μL, 0.69 mmol). The resultant mixture was stirred for 24 h at room temperature. The reaction mixture was extracted with CH2Cl2 (15 mL) and water (10 mL). The organic solution was passed through a hydrophobic frit and the solvent was removed in vacuo. Purification by SPE (5 g Silica cartridge) eluted with 1:49–1:19 EtOAc:cyclohexane afforded the title compound as a white crystalline solid (76 mg).

1. extractionThe reaction mixture was extracted with CH2Cl2 (15 mL) and water (10 mL)
2. customthe solvent was removed in vacuo
3. customPurification by SPE (5 g Silica cartridge)
4. washeluted with 1:49–1:19 EtOAc

ORDレコード

ord-be80d91fa8f54f4bba68b342fb5966ea

出典データセット

uspto-grants-2007_04

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07199239B2