HRID717547

反应详情

EQUATION

反应方程式

HRID 717547 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2,4,6-trimethylbenzenesulfonyl chloride (5 g, 0.022 mol) was added to a solution of methyl tertiary-butyl ether (50 mL) under nitrogen atmosphere at 0° C., followed by the addition of tert-butyl hydroxycarbamate (3.04 g, 0.22 mol) at 0° C. Next, triethylamine (3.24 mL, 0.023 mol) was added drop wise to the reaction mixture, which was then it was allowed to stir for 2 h. The reaction product was filtered through sintered funnel and the filtrate was concentrated under vacuum up to ¾ volume. Hexane (50 mL) was added to the concentrated filtrate, which was then stirred for 20 min wherein a precipitate formed. The participate was collected by filtration and the solid dried to afford tert-butyl(mesitylsulfonyl)oxycarbamate. 1H NMR (400 MHz, CDCl3) δ 8.49 (s, 1H), 8.31 (s, 1H), 2.38 (s, 9H). MS (M+1): 316.3.

WORKUP

后处理

  1. filtrationThe reaction product was filtered through sintered funnel
  2. concentrationthe filtrate was concentrated under vacuum up
  3. additionHexane (50 mL) was added to the concentrated filtrate, which
  4. stirringwas then stirred for 20 min wherein a precipitate
  5. customformed
  6. filtrationThe participate was collected by filtration
  7. customthe solid dried