HRID929399

反应详情

EQUATION

反应方程式

HRID 929399 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-Chloroadenine (10.0 g, 59 mmol), butylamine (43 mL, 589 mmol) and water (40 mL) were placed in an autoclave (250 mL), and the content of the autoclave was allowed to react at 180° C. for 18 h. The reaction solution was concentrated under reduced pressure, and water was poured into the residue to precipitate a solid. The precipitated solid was sequentially washed with water, EtOH and acetone. Thus, 10.39 g of the title compound was obtained as a yellowish orange powdery solid (yield: 86%). Intermediate 1 was characterized by the following spectroscopic data: 1H NMR (DMSO-d6, 300 MHz): 11.92 (br. S, 1H), 7.63 (s, 1H), 6.51 (br. s, 2H), 6.04 (s, 1H), 3.19 (q, 2H), 1.51 (m, 2H), 1.33 (m, 2H), 0.92 (t, 3H).

WORKUP

后处理

  1. customto react at 180° C. for 18 h
  2. concentrationThe reaction solution was concentrated under reduced pressure, and water
  3. additionwas poured into the residue
  4. customto precipitate a solid
  5. washThe precipitated solid was sequentially washed with water, EtOH and acetone