HRID909259

反应详情

EQUATION

反应方程式

HRID 909259 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
40 °C

PROCEDURE

实验过程

A mixture of 32.6 mg (0.1 mmol) trans-(4-amino-cyclohexyl)-(4-isopropyl-piperazin-1-yl)-methanone, dihydrochloride, 28 mg (0.2 mmol) propane-1-sulfonyl chloride and 101 mg (1 mmol) NEt3 in 2 ml DCM was stirred for 16 h at 40° C. After evaporation methanol and DMF were added and the mixture was subjected to preparative HPLC purification on reversed phase eluting with a gradient of acetonitrile/water (0.1% NEt3). The combined product fractions were evaporated to dryness to yield 13.9 mg (39%) of the title compound. MS (m/e): 360.4 (MH+).

WORKUP

后处理

  1. customAfter evaporation methanol and DMF
  2. additionwere added
  3. customthe mixture was subjected to preparative HPLC purification on reversed phase
  4. washeluting with a gradient of acetonitrile/water (0.1% NEt3)
  5. customThe combined product fractions were evaporated to dryness