反应 #413676

ord-c8b43c17951f49419a5b86a9797bd07c

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他The reaction is partitioned between ether and aqueous sodium bicarbonate
  2. 2
    洗涤The organic phase is washed with saline
  3. 3
    干燥dried over sodium sulfate
  4. 4
    浓缩concentrated
  5. 5
    其他The residue is chromatographed on silica gel with methanol/methylene chloride (4/96)

实验过程

17α-Hydroxy-21-iodopregna-4,9(11)-diene-3,20-dione (4.53 g) is stirred in acetonitrile (50 ml) with 1-(2-pyridinyl)piperazine (1.63 g) and potassium carbonate (1.34 g) at 60° for 5 hr and at 20°-25° for 17 hr. The reaction is partitioned between ether and aqueous sodium bicarbonate. The organic phase is washed with saline, dried over sodium sulfate and concentrated. The residue is chromatographed on silica gel with methanol/methylene chloride (4/96) to give the title compound.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05268477uspto-grants-1993_12