反应 #594582

ord-709ed9e2e3aa42eca8d1d7a6c62ef17a

反应条件

温度
50°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他is separated
  2. 2
    其他dried
  3. 3
    其他evaporated
  4. 4
    其他The residue is purified by preparative HPLC (Method 1)

实验过程

3-[2-(4-Amino-phenyl)-ethyl]-2-methyl-5,5-diphenyl-3,5-dihydro-imidazol-4-one (56 mg, 0.15 mmol) is dissolved in 10 mL methylene chloride and 2-ethyl-butyric acid (18 mg, 0.15 mmol), bromo-tris-pyrrolidino-phosphonium hexafluorophosphate (113 mg, 0.24 mmol) and ethyl diisopropyl amine (42 uL, 0.24 mmol) are added. The mixture is stirred and heated to 50° C. for 5 hours. Subsequently water and methylene chloride are added the organic phase is separated, dried and evaporated. The residue is purified by preparative HPLC (Method 1) to yield 2-ethyl-N-{4-[2-(2-methyl-5-oxo-4,4-diphenyl-4,5-dihydro-imidazol-1-yl)-ethyl]-phenyl}-butyramide (25 mg, 35%). LC/MS at 254 nm; [M+H] 468; Rt 3.351.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07786155B2uspto-grants-2010_08