HRID535477

反应详情

EQUATION

反应方程式

HRID 535477 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 4-chlorophthalazin-1-one (0.49 g, 2.7 mmol), morpholine (2.4 mL, 27 mmol), and ethylene glycol (1.5 mL) was microwaved at 190° C. for 1 hour, and 210° C. for 30 minutes, diluted with EtOAc, washed with sat NaHCO3 and water, concentrated, adsorbed onto silica, and chromatographed (30% EtOAc/DCM) to give 300.0 mg of product as a white solid: 1H NMR (300 MHz, DMSO-d6) δ 12.13 (s, 1H), 8.27-8.20 (m, 1H), 8.00-7.79 (m, 3H), 3.86-3.77 (m, 4H), 3.07 (dd, J=10.2, 5.6, 4H).

WORKUP

后处理

  1. customwas microwaved at 190° C. for 1 hour
  2. washwashed
  3. concentrationconcentrated
  4. customchromatographed (30% EtOAc/DCM)