HRID1638529

反应详情

EQUATION

反应方程式

HRID 1638529 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Compound 9 (1.0 g, 1.63 mmol) was combined with methanolic ammonia (saturated at 0° C., 50 mL) and heated at 90° C. for 14 h in a steel bomb. The solvent was evaporated and the residue was treated with hot benzene which was decanted off. The resulting solid was purified by silica gel flash chromatography using chloroform and then CHCl3 --MeOH (6:1) to yield 280 mg (57%) of 10 after crystallization from water: mp 216°-218° C.: UV λmax (pH 1) 217 nm (ε25300), 259 (9700), 286 (6300): 1H NMR (DMSO-d6) δ5.85 (d, J=5.1 Hz, 1H, C1, H), 8.30 (s, 1H, C5H), 13.09 (b, 1H, N6H, exchanges with D2O), and other sugar protons. Anal. Calcd. for C10H11N3O 6 S: C, 39.87: H, 3.68: N, 13.95: S, 10.64. 3.61: N, 14.06: S, 10.43.

WORKUP

后处理

  1. customThe solvent was evaporated
  2. additionthe residue was treated with hot benzene which
  3. customwas decanted off
  4. customThe resulting solid was purified by silica gel flash chromatography