HRID389553

反应详情

EQUATION

反应方程式

HRID 389553 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 2-(thieno[2,3-d]pyridazin-3-yl)furo[2,3-c]pyridin-7-amine (30.0 mg, 0.112 mmol) and N-iodosuccinimide (101.6 mg, 0.4516 mmol) in N,N-dimethylformamide (2 mL) was stirred at 40° C. for 45 min. The reaction was removed from the heat and 1.0 M aqueous sodium thiosulfate solution (2 mL) was added. The crude mixture was concentrated in vacuo. The residue was then suspended in water and the fine solid was filtered off and dried, giving 39.0 mg (88%) of the title compound as a brown solid. 1H NMR (400 MHz, DMSO-d6): δ 10.48 (d, J=1.52 Hz, 1H), 10.02 (d, J=1.52 Hz, 1H), 9.04 (s, 1H), 7.96 (s, 1H), 7.45 (s, 1H), 6.89 (s, 2H); MS (ESI): 395.07 [M+H]+; HPLC: tR=2.83 min.

WORKUP

后处理

  1. customThe reaction was removed from the
  2. temperatureheat
  3. addition1.0 M aqueous sodium thiosulfate solution (2 mL) was added
  4. concentrationThe crude mixture was concentrated in vacuo
  5. filtrationthe fine solid was filtered off
  6. customdried