HRID1711044

反应详情

EQUATION

反应方程式

HRID 1711044 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Starting from the compound 268 and following the procedure described above for the synthesis of compound 269a (example 221) but replacing 2-phenylacethyl isothiocyanate with 2-(2,6-dichlorophenyl)acetyl isothiocyanate, a white solid was obtained. This material was dissolved in MeOH and treated with HCl (1 mL, 1.0M in ether). Solvents were removed under the reduced pressure and the residue was lyophilized, to afford the title compound 269b (48% yield) as a yellowish solid. 1H NMR (DMSO-d6) δ (ppm): 13.29 (s, 1H), 12.32 (s, 1H), 12.05(s, 1H), 8.52(d, 1H), 8.14 (m, 2H), 7.64 (m, 2H), 7.51(d, 1H), 7.37(dd, 1H), 6.86 (m, 1H), 6.81(dd, 1H), 4.22 (s, 2H), MS (m/z): 489.1 (M+H) (found).

WORKUP

后处理

  1. customa white solid was obtained
  2. customSolvents were removed under the reduced pressure