HRID2252036

反应详情

EQUATION

反应方程式

HRID 2252036 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 2-phenyl-6,7-dihydro-5H-pyrrolo[1,2-a]imidazole (3.38 g, 18.3 mmol) in dry CH2Cl2 (113 mL) slowly add bromine (1.0 mL, 20.2 mmol) and stir the mixture at room temperature for 1.5 hours. Add a saturated aqueous solution of NaHCO3 (100 mL) and extract with CH2Cl2 (3×100 mL). Wash the combined organic layers with NaHSO3 (40%, 30 mL), dry (MgSO4) and concentrate in vacuo. Purify the residue by flash chromatography (SiO2, eluent: CH2Cl2 to CH2Cl2/MeOH 20:1) to yield a red solid, 3.54 g, 73% yield. MS(ES+): m/z=263.0 (M+H)+

WORKUP

后处理

  1. extractionextract with CH2Cl2 (3×100 mL)
  2. washWash the combined organic layers with NaHSO3 (40%, 30 mL)
  3. dry with materialdry (MgSO4)
  4. concentrationconcentrate in vacuo
  5. customPurify the residue by flash chromatography (SiO2, eluent: CH2Cl2 to CH2Cl2/MeOH 20:1)
  6. customto yield a red solid, 3.54 g, 73% yield