HRID1372253

反应详情

EQUATION

反应方程式

HRID 1372253 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Intermediate 100, 2-(1,1-dioxo-1λ6-[1,2]thiazinan-2-yl)benzonitrile, (2.63 g, 11.14 mmol) was dissolved in ethanol (150 mL) and 1N HCl (13 mL). Added to this was 10% Pd—C (0.5 g) and the mixture shaken under H2 at 55 psi for 24 h. Filtration through Celite followed by concentration gave the title compound as a white solid (2.93 g, 95% yield). 1H-NMR (300 MHz, CD3OD) δ ppm: 7.61–7.47 (4H, m), 4.30 (2H, q, J=13.7 Hz), 3.96–3.87 (1H, m), 3.49–3.36 (3H, m), 2.40–2.31 (2H, m), 2.05–1.96 (2H, m). LCMS [M+H]+ calcd for C11H17N2SO2: 241.10. found: 241.10.

WORKUP

后处理

  1. filtrationFiltration through Celite
  2. concentrationfollowed by concentration