HRID2079860

反应详情

EQUATION

反应方程式

HRID 2079860 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

5% Pd/C (30 mg) was wetted carefully with methanol under nitrogen in a 25 ml round flask, then a solution of 5-(4,6-bis-benzyloxy-5′-isopropyl-2′-methoxy-biphenyl-3-yl)-1-phenethyl-1H-tetrazole (100 mg, 0.16 mmol) in methanol (10 ml) was added. The reaction flask was vacuumed and filled with hydrogen three times. The reaction was then stiffed under hydrogen at r.t. overnight. After filtering the catalyst over celite, the filtrate was concentrated to give 5′-isopropyl-2′-methoxy-5-(1-phenethyl-1H-tetrazol-5-yl)-biphenyl-2,4-diol (44 mg, 63%). M.p.: 206-209° C.; 400 MHz 1H NMR (DMSO-d) δ: 10.22 (s, 1H), 9.64 (s, 1H), 7.19-7.08 (m, 4H), 7.02-6.97 (m, 3H), 6.94 (d, J=8.4 Hz, 1H), 6.75 (s, 1H), 6.61 (s, 1H), 4.55 (t, J=7.2 Hz, 2H), 3.66 (s, 3H), 3.11 (t, J=7.2 Hz, 2H), 2.90-2.81 (m, 1H), 1.20 (d, J=7.2 Hz, 6H); LCMS: 431 [M+H].

WORKUP

后处理

  1. filtrationAfter filtering the catalyst over celite
  2. concentrationthe filtrate was concentrated