HRID1824650

反应详情

EQUATION

反应方程式

HRID 1824650 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Acenaphtho[1,2-b]quinoxaline (10 g) was charged into 10% oleum (49 ml), stirredfor 30 minutes and heated at 180–190° C. for 30 hours. The reaction mixture was then diluted with water (95 ml), and the formed precipitate was filtered and washed with acetic acid (˜30 ml). The filtered cake was dried on air at 120° C. to yield 8.2 g of acenaphtho[1,2-b]quinoxaline-2,5-disulfonic acid. 1H NMR (Bruker AMX-400, DMSO-d6, δ, ppm): 7.82 (q, 2H, 3 Hz); 8.18 (q, 2H, 3 Hz); 8.24–8.36 (broad s, 2H); 8.62 (s, 4H). Elemental analysis calculated for C18H10N2O6S2: C, 52.17; H, 2.43; N, 6.76; found: C, 52.02; H, 2.35; N, 6.56.

WORKUP

后处理

  1. temperatureheated at 180–190° C. for 30 hours
  2. filtrationthe formed precipitate was filtered
  3. washwashed with acetic acid (˜30 ml)
  4. customThe filtered cake was dried on air at 120° C.