HRID2356049

反应详情

EQUATION

反应方程式

HRID 2356049 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of methyl-3-nitro-1-nitrosoguanidine (1.18 g, 8.1 mmol), 40% KOH (3.4 mL), and diethyl ether (12 mL) at 0° C. was stirred for 10 minutes. The organic phase was added slowly to a −25° C. solution of Example 158C and Pd(OAc)2 (18 mg, 0.11 mmol) in THF (8.8 mL). The mixture was stirred for 1 hour at −20° C. and concentrated. The concentrate was purified by flash column chromatography on silica gel with 9:1 hexanes/ethyl acetate to provide the desired product. MS (DCI) m/e 260 (M+H)+.

WORKUP

后处理

  1. stirringThe mixture was stirred for 1 hour at −20° C.
  2. concentrationconcentrated
  3. customThe concentrate was purified by flash column chromatography on silica gel with 9:1 hexanes/ethyl acetate