HRID235525
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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): δ1.45 (t, 2H), 1.60 (m, 4H), 2.55-2.75 (4H), 3.40 (m, 2H), 3.55 (br, 1H), 3.74-3.96 (8H), 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
- additionwas added
- customThe solvent was removed
- customthe crude product chromatographed on silica gel
- washeluting with 2% and 5% methanol in methylene chloride
- customThe solvent was removed
- customthe product dried