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
Into a Round bottom flask, 7-Bromo-2-methylsulfanyl-pyrrolo[2,1-f][1,2,4]triazine (4.00 g, 0.0164 mol) and Methylene chloride (100 mL) were added. m-Chloroperbenzoic acid (77% max)(5.14 g, 0.0229 mol) was added portion wise over 20 minutes and the reaction was stirred at room temperature for one hour. The mixture was partitioned with DCM (200 mL) and saturated NaHCO3 (200 mL). Organic extracts were washed with Brine and dried over Na2SO4. The solid was filtered and washed with DCM. The solvent was removed under vacuum to give a yellow solid. The solid was washed with hexane to afford 3.27 grams of 7-Bromo-2-methanesulfinyl-pyrrolo[2,1-f][1,2,4]triazine as a yellow powder. 1H NMR (400 MHz, DMSO, d6) δ 9.34 (s, 1H), 7.51 (m, 1H), 7.41 (d, 1H, J=4.71 Hz), 3.43 (s, 3H).
WORKUP
后处理
- customThe mixture was partitioned with DCM (200 mL) and saturated NaHCO3 (200 mL)
- washOrganic extracts were washed with Brine
- dry with materialdried over Na2SO4
- filtrationThe solid was filtered
- washwashed with DCM
- customThe solvent was removed under vacuum
- customto give a yellow solid
- washThe solid was washed with hexane