反应 #3329302
相关文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US09290459B1
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 3-(3-(Trifluoromethyl)phenylamino)cyclopent-2-enone (234 mg, 0.97 mmol) is added to a solution of 4-bromo-1-(chloro(isocyanato)methyl)-2-(methylsulfonyl)benzene (Step 1, 945 mg, 2.91 mmol) in dichloromethane (10 mL). The mixture is heated at reflux over night and then concentrated under reduced pressure. The residue is purified by reversed phase HPLC (Agilent ZORBAX™ SB—C18, gradient of acetonitrile in water, 0.1% formic acid). Yield: 110 mg; ESI mass spectrum: ESI mass spectrum: [(79Br)-M+H]+=529, [(81Br)-M+H]+=531; Retention time HPLC: 1.21 min (Z017_S04). The mixture is heated at reflux over night concentrated under reduced pressure The residue is purified by reversed phase HPLC (Agilent ZORBAX™ SB—C18, gradient of acetonitrile in water, 0.1% formic acid) 1.21 min (Z017_S04)
来源 ID: ord-d1c1d80ae4bc45a7aa95938feeec1b47