反应 #2487492

ord-23afe677a3ce404b85fdfcba67b7f367

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他the solution was placed in an ice bath
  2. 2
    其他The solvent was removed under vacuum
  3. 3
    其他the residue was partitioned between AcOEt (25 ml) and 5% AcOH (15 ml)
  4. 4
    洗涤The organic phase was washed with 5% AcOH (2×15 ml), and saturated NaHCO3
  5. 5
    其他dried
  6. 6
    浓缩concentrated under vacuum

实验过程

(S)-2-[12-(4-tert-Butoxycarbonylphenyl) dodecanoylamino]pentanedioic acid 1-tert-butyl ester (158 mg, 0.28 mmol) was dissolved in THF (6 ml). DIEA (48 μl, 0.28 mmol) was added, and the solution was placed in an ice bath. HSTU (101 mg, 0.28 mmol) was added, and the solution was stirred for 16 h, warming to rt slowly. The solvent was removed under vacuum, and the residue was partitioned between AcOEt (25 ml) and 5% AcOH (15 ml). The organic phase was washed with 5% AcOH (2×15 ml), and saturated NaHCO3, dried, and concentrated under vacuum to yield an oil (0.16 g).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08796205B2uspto-grants-2014_08