HRID853798

反应详情

EQUATION

反应方程式

HRID 853798 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 5-hydroxy-2-(4-hydroxyphenyl)isoindoline-1,3-dione (2.08 g) in DMF (20 mL) was added potassium carbonate (4.62 g) and a solution of benzyl bromide (3.07 g) in DMF (3.0 mL) dropwise under nitrogen atmosphere. The reaction was stirred at room temperature for 2 h then heated to 80° C. for 3 h. The mixture was cooled to room temperature, poured into water (250 mL) and let sit undisturbed for 2.0 h. The white solid was collected by filtration and washed with water. The solid was dried under high vacuum at 50° C. for 18 h yielding the title compound (3.30 g) as a white solid. 1H NMR (DMSO-d6): 7.87 (d, 1H, J=8.4 Hz), 7.48-7.35 (m, 12H), 7.32 (d, 2H, J=8.7 Hz), 7.13 (d, 2H, J=8.7 Hz), 5.35 (s, 2H), 5.17 (s, 2H); MS: 436 (MH+).

WORKUP

后处理

  1. temperaturethen heated to 80° C. for 3 h
  2. temperatureThe mixture was cooled to room temperature
  3. waitlet sit undisturbed for 2.0 h
  4. filtrationThe white solid was collected by filtration
  5. washwashed with water
  6. customThe solid was dried under high vacuum at 50° C. for 18 h