HRID2238447

反应详情

EQUATION

反应方程式

HRID 2238447 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 225 (1.17 g, 3.02 mmol) in MeOH (30 mL) with Pd/C (5%, 0.21 g) was hydrogenated at 50 psi for 2.5 h. The mixture was filtered through Celite, washing with MeOH, and the filtrate was evaporated. The residue was dissolved in CH2Cl and the solution was filtered once more, then evaporated to give 2-aminoethyl di(tert-butyl) phosphate (226) (604 mg, 79%) as a colourless oil: 1H NMR [CDCl3] δ 4.01-3.94 (m, 2H), 2.96-2.90 (m, 2H), 1.58 (br s, 2H), 1.49 (s, 18H). HRMS (FAB) calcd. for C10H25NO4P (MH+) m/z 254.1521, found 254.1519.

WORKUP

后处理

  1. filtrationThe mixture was filtered through Celite
  2. washwashing with MeOH
  3. customthe filtrate was evaporated
  4. dissolutionThe residue was dissolved in CH2Cl
  5. filtrationthe solution was filtered once more
  6. customevaporated