HRID52849

反应详情

EQUATION

反应方程式

HRID 52849 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A 0.170 g (0.237 mmol) of the compound from Example 337B above was dissolved in 2 mL of methanol to which 30 μL of trimethylsilyl chloride was added and stirred for 2.25 hours. The solvent was removed and the crude product chromatographed on silica gel, eluting with 2% and 5% methanol in methylene chloride. The solvent was removed and the product dried to afford 22.7 mg of the title compound. MS M/Z (DCI/NH3): 489 (M+H), 506 (M+NH4). Proton NMR (DMSO): δ 1.45 (t, 2H), 1.60 (m, 4H), 2.55-2.75 (4H), 3.40 (m, 2H), 3.55 (br, 1H), 3.74-3.96 (18H), 4.44 (t, 2H), 4.62 (d, 1H), 6.63 (d, 1H), 6.89 (d, 1H), 7.07-7.27 (10H).

WORKUP

后处理

  1. additionwas added
  2. customThe solvent was removed
  3. customthe crude product chromatographed on silica gel
  4. washeluting with 2% and 5% methanol in methylene chloride
  5. customThe solvent was removed
  6. customthe product dried