HRID220558

反应详情

EQUATION

反应方程式

HRID 220558 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Add 2-(4-bromo-phenyl)-acetyl chloride (1.00 g, 4.28 mmol) to a solution of ammonia in dioxane (0.5 M, 15 mL) at room temperature. Stir for 30 min., then quench with water. Extract with DCM (10 mL) and pass through an IST Phase Separator Frit® and concentrate until precipitate appears. Collect precipitate by filtration, wash powder with DCM, then dissolve in methanol, filter and concentrate to give a white powder (1.0 g, 109%). 1H-NMR (300 MHz, MeOD) δ 7.48 (d, 2H), 7.25 (d, 2H), 3.50 (s, 2H).

WORKUP

后处理

  1. customquench with water
  2. extractionExtract with DCM (10 mL)
  3. concentrationconcentrate until precipitate appears
  4. customCollect precipitate
  5. filtrationby filtration
  6. washwash powder with DCM
  7. dissolutiondissolve in methanol
  8. filtrationfilter
  9. concentrationconcentrate