HRID1261936

反应详情

EQUATION

反应方程式

HRID 1261936 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customThe mixture was partitioned with DCM (200 mL) and saturated NaHCO3 (200 mL)
  2. washOrganic extracts were washed with Brine
  3. dry with materialdried over Na2SO4
  4. filtrationThe solid was filtered
  5. washwashed with DCM
  6. customThe solvent was removed under vacuum
  7. customto give a yellow solid
  8. washThe solid was washed with hexane