HRID518738

反应详情

EQUATION

反应方程式

HRID 518738 的结构方程式

PROCEDURE

实验过程

A suspension of cis-4-(5-chloro-2-nitrophenylamino)-N-isopropylcyclohexanecarboxamide (300 mg, 0.883 mmol) in morpholine (2 mL, 22.93 mmol) was irradiated in a microwave reactor for 1 hour at 150° C. The reaction mixture was partitioned between water and DCM. The organic layer was dried over anhydrous magnesium sulfate, filtered, and concentrated to a yellow oil. The residue was concentrated, adsorbed onto a plug of silica gel, and purified by column chromatography, eluting with 0-100% EtOAc in DCM, to provide cis-N-isopropyl-4-(5-morpholino-2-nitrophenylamino)cyclohexanecarboxamide as a yellow powder (0.38 g, 110% yield). MS, m/z (C20H30N4O4): calcd, 390.2. found, 390.9 [M+H].

WORKUP

后处理

  1. customwas irradiated in a microwave reactor for 1 hour at 150° C
  2. customThe reaction mixture was partitioned between water and DCM
  3. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated to a yellow oil
  6. concentrationThe residue was concentrated
  7. custompurified by column chromatography
  8. washeluting with 0-100% EtOAc in DCM