HRID1366562
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a solution of (9aR)-8-(phenylmethyl)octahydropyrazino[2,1-c][1,4]oxazine (1.8055 g, 7.77 mmol) in MeOH (80 mL) was added 1 N aq. HCl (15.5 mL, 15.5 mmol) and 10% Pd/C (50% water, 360 mg). The mixture was hydrogenated under balloon pressure overnight, and was then filtered through a 0.2 μm PTFE membrane. The solution was concentrated in vacuo and the residue was azeotroped with MeOH (3×50 mL) to provide crude (9aR)-octahydropyrazino[2,1-c][1,4]oxazine dihydrochloride (1.7185 g, >100% crude yield) as an orange solid. LCMS: (M+H)+: 142.9.
WORKUP
后处理
- customwas hydrogenated under balloon pressure overnight
- filtrationwas then filtered through a 0.2 μm PTFE membrane
- concentrationThe solution was concentrated in vacuo
- customthe residue was azeotroped with MeOH (3×50 mL)