HRID548263

反应详情

EQUATION

反应方程式

HRID 548263 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

(4-Hydroxymethyl-benzyl)-carbamic acid tert-butyl ester (480 mg, 0.71 mmol) was dissolved in DCM (3 mL) and cooled to −78° C. (dry ice/acetone). Dess-Martin periodinane (331 mg, 0.78 mmol) was added to the reaction which was allowed to warm to r.t and stir for 3 h. A 1:1 solution of saturated sodium bicarbonate and sodium sulfite (20 mL) was added and the reaction mixture stirred vigorously for 15 min. The organic layer was isolated, washed with saturated sodium bicarbonate (10 mL), dried (Na2SO4) and evaporated to dryness to afford the desired compound (480 mg, 100%). m/z 258 [M++Na]+

WORKUP

后处理

  1. temperatureto warm
  2. stirringthe reaction mixture stirred vigorously for 15 min
  3. customThe organic layer was isolated
  4. washwashed with saturated sodium bicarbonate (10 mL)
  5. dry with materialdried (Na2SO4)
  6. customevaporated to dryness