HRID75847

反应详情

EQUATION

反应方程式

HRID 75847 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To Methyl 2-(3-(4-(benzyloxy)phenyl)isoxazole-5-carboxamido)-3-methylbutanoate (6 g) in THF (120 ml), 10% Palladium on carbon (Wet, 600 mg) was added and hydrogenated at 50 psi for 3 hours. Reaction mixture was filtered through Celite and filtrate was concentrated to obtain yellow residue. This residue was purified by column chromatography (silica gel, EtOAc—CHCl3) to obtain yellow solid, which was crystallized using DCM—Petroleum ether to obtain the title compound as pale yellow solid. Yield: 2.25 g (48%); MS (ES+): m/z−319 (M+1); 1HNMR (DMSO-d6; 300 MHz): δ 10.01 (bs, 1H), 9.16 (d, 1H), 7.75 (d, 2H), 7.61 (s, 1H), 6.91 (d, 2H), 4.3 (m, 1H), 3.67 (s, 3H), 2.21 (m, 1H), 0.96 (d, 6H);

WORKUP

后处理

  1. customReaction mixture
  2. filtrationwas filtered through Celite and filtrate
  3. concentrationwas concentrated
  4. customto obtain yellow residue
  5. customThis residue was purified by column chromatography (silica gel, EtOAc—CHCl3)
  6. customto obtain yellow solid, which
  7. customwas crystallized