HRID2228417

反应详情

EQUATION

反应方程式

HRID 2228417 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Phytanyl bromide (12.34 g), potassium phthalimide (6.95 g) and DMF (50 ml) were heated at 120-130° C. for 4 hours. Most of the DMF was removed under reduced pressure and the crude product was dissolved in dichloromethane (100 ml), washed with water (2×50 ml), dried (MgSO4). The light yellow crude product was chromatographed on flash silica (dichloromethane/hexane as eluant) to yield pure N-phytanyl phthalimide in 11.89 g (80.9%) 1H-n.m.r. (CDCl3) δ0.82-1.8 (m, 39H), 3.73 (t, 2H, CH2N), 7.73 (m, 2H, ArH), 7.88 (m, 2H, ArH); m/z 431 (M+).

WORKUP

后处理

  1. customMost of the DMF was removed under reduced pressure
  2. dissolutionthe crude product was dissolved in dichloromethane (100 ml)
  3. washwashed with water (2×50 ml)
  4. dry with materialdried (MgSO4)
  5. customThe light yellow crude product was chromatographed on flash silica (dichloromethane/hexane as eluant)