HRID220558
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customquench with water
- extractionExtract with DCM (10 mL)
- concentrationconcentrate until precipitate appears
- customCollect precipitate
- filtrationby filtration
- washwash powder with DCM
- dissolutiondissolve in methanol
- filtrationfilter
- concentrationconcentrate