HRID450372

反应详情

EQUATION

反应方程式

HRID 450372 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of (RS)—N-[(1R)-2-{[tert-butyl(dimethyl)silyl]oxy}-1-(5-fluoropyridin-2-yl)ethyl]-2-methylpropane-2-sulfinamide (Intermediate 22, 1.13 g, 3.02 mmol) in MeOH (15 ml) was added hydrochloric acid (4 M in dioxane, 3.02 ml, 12.08 mol) at 0° C. and the mixture was stirred for 15 minutes and was concentrated. The mixture was triturated from hexanes to provide the title salt (575 mg). The product is highly hygroscopic. 1H NMR (300 MHz, DMSO-d6) δ ppm 8.62 (s, 1H) 8.55 (s, 2H) 7.76-7.93 (m, 1H) 7.65 (dd, J=8.29, 4.52 Hz, 1H) 4.43 (d, J=4.52 Hz, 1H) 3.77 (s, 2H).

WORKUP

后处理

  1. concentrationwas concentrated
  2. customThe mixture was triturated from hexanes