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

To a solution of N-butyl-N-[4′-(trifluoromethyl)-1,1′-biphenyl-3-yl]amine (0.128 g, 0.44 mmol) In anhydrous CH2Cl2 (10 mL) was added ethyl [4-(chlorosulfonyl)-2-methylphenoxy]acetate (0.121 g, 0.41 mmol) and triethylamine (0.122 mL, 0.87 mmol). The resultant mixture was stirred for 24 h at room temperature prior to addition of sulfonyl chloride (0.121 mg, 0.41 mmol) and triethylamine (0.122 mL, 0.87 mmol). After a further 18 h stirring at room temperature the reaction was diluted with water (10 mL) and extracted with CH2Cl2 (2×10 mL). The organic solution was dried (Na2SO4) and the solvents removed in vacuo. Purification by SPE (Silica, 10 g) eluting 49:1–19:1 cyclohexane:EtOAc afforded the title compound as a pale yellow oil (0.182 g).

1. extractionextracted with CH2Cl2 (2×10 mL)
2. dry with materialThe organic solution was dried (Na2SO4)
3. customthe solvents removed in vacuo
4. customPurification by SPE (Silica, 10 g)
5. washeluting 49:1–19:1 cyclohexane

ORDレコード

ord-8a78a4cff166489eb3f838fd61bb35d4

出典データセット

uspto-grants-2007_04

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07199239B2