HRID1095472

反应详情

EQUATION

反应方程式

HRID 1095472 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of N-(4-aminophenethyl)-5,6-diphenylfuro[2,3-d]pyrimidin-4-amine (0.195 g) in acetonitrile (10 mL) was added phenyl isocyanate (0.063 g). After stirring at room temperature for 16 h, the reaction mixture was concentrated and the residue was partitioned between water and ethyl acetate. The organic layer was concentrated and the crude compound was purified by silica gel column chromatography using a mixture of hexanes:ethyl acetate (1:1), to give 1-(4-(2-(5,6-diphenylfuro[2,3-d]pyrimidin-4-ylamino)ethyl)phenyl)-3-phenylurea (0.240 g, 95%). 1H-NMR (CDCl3, 300 MHz): δ 8.42 (s, 1 H), 7.58 (brs, 1 H), 7.43-7.39 (m, 5 H), 7.33-7.18 (m, 11 H), 7.03-6.98 (m, 1 H), 6.86-6.83 (m, 2 H), 4.67 (t, 1 H), 3.63 (q, 2 H), 2.66 (t, 2 H). LC-MS (ESI) m/z 526.2 (M+H).

WORKUP

后处理

  1. concentrationthe reaction mixture was concentrated
  2. customthe residue was partitioned between water and ethyl acetate
  3. concentrationThe organic layer was concentrated
  4. customthe crude compound was purified by silica gel column chromatography
  5. additiona mixture of hexanes:ethyl acetate (1:1)