HRID2238447
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- filtrationThe mixture was filtered through Celite
- washwashing with MeOH
- customthe filtrate was evaporated
- dissolutionThe residue was dissolved in CH2Cl
- filtrationthe solution was filtered once more
- customevaporated