HRID423328

反应详情

EQUATION

反应方程式

HRID 423328 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 5-(5-{3-chloro-4-[(1-methylethyl)oxy]phenyl}-1,2,4-oxadiazol-3-yl)-1H-indole (D5) (450 mg, 1.27 mmol) dissolved in DMF (12 ml) was added bromine (213 mg, 1.35 mmol) dropwise. Stirred for 15 minutes, evaporated off the DMF, added diethyl ether (70 ml) and washed with water (2×70 ml). Dried over MgSO4 and evaporated off the solvent. The residue was crystallised from diethyl ether/hexane to give 160 mg of the title compound as a white solid. δH (400 MHz, d6-DMSO) 1.37 (6H, d), 4.88 (1H, sept), 7.44 (1H, d), 7.59 (1H, dd), 7.72 (1H, d), 7.91 (1H, dd), 8.13-8.32 (3H, m). MS (ES) C19H1579BrClN3O2 requires 431; found 432 (MH+).

WORKUP

后处理

  1. customevaporated off the DMF
  2. additionadded diethyl ether (70 ml)
  3. washwashed with water (2×70 ml)
  4. dry with materialDried over MgSO4
  5. customevaporated off the solvent
  6. customThe residue was crystallised from diethyl ether/hexane