HRID243323

反应详情

EQUATION

反应方程式

HRID 243323 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
130 °C

PROCEDURE

实验过程

Into a 25-mL round-bottom flask was placed a solution of (S)-1-(1-phenyl-1H-benzo[d]imidazol-2-yl)ethanamine from Example 4 (238 mg, 1.00 mmol, 1.00 equiv) in n-BuOH (8 mL), 6-chloro-9H-purin-2-amine (155 mg, 0.91 mmol, 0.91 equiv, 98%) and N-ethyl-N-isopropylpropan-2-amine (390 mg, 2.96 mmol, 2.95 equiv, 98%). The resulting solution was stirred overnight at 130° C. and concentrated under vacuum. The residue was eluted onto a C18 column (water/acetonitrile) to afford 0.150 g (40%) of 149 as a white solid. LC-MS (ES, m/z): 371 [M+H]+. H-NMR (300 MHz, CD3OD, ppm): δ 7.71 (d, 2H), 7.51 (s, 5H), 7.29 (m, 2H), 7.10 (d, 1H), 5.67 (s, 1H), 1.69 (d, 3H)

WORKUP

后处理

  1. customInto a 25-mL round-bottom flask was placed
  2. concentrationconcentrated under vacuum
  3. washThe residue was eluted onto a C18 column (water/acetonitrile)