HRID1047101

反应详情

EQUATION

反应方程式

HRID 1047101 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a stirred solution of trityl acid 8 (280 mg, 0.42 mM) in dry THF (6 mL) was added dicyclohexyl carbodiimide (DDC, 400 mg, 1.95 mM). The reaction mixture was stirred for 30 min at r.t., maleimide (100 mg, 1.1 mM) and a catalytic amount of DMAP were added and allowed to stir for overnight. The solvent was removed under rotaevaporator and the solid obtained was dissolved in dry ether. The precipitated DCU was filtered and the solvent ether was evaporated. Part of the product was purified by preparative TLC. Yield: 12 mg. 1H-NMR (500 MHz, CDCl3) δ ppm: 1.78 (m, 2H), 1.95 (m 2H), 2.9 (s, 4H), 3.51 (m, 2H), 3.93 (t, 2H), 4.02 (t, 2H), 6.8 (m, 5H), 7.25 (m, 5H), 7.29 (m, 5H), 7.37 (m, 3H), 7.48 (d, 2H), Mass: 561.3 (M+).

WORKUP

后处理

  1. stirringto stir for overnight
  2. customThe solvent was removed under rotaevaporator
  3. customthe solid obtained
  4. filtrationThe precipitated DCU was filtered
  5. customthe solvent ether was evaporated
  6. customPart of the product was purified by preparative TLC