HRID16187
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
CONDITIONS
反应条件
- 温度
- 65 °C
PROCEDURE
实验过程
To a solution of ethyl trans-[(7-chloro-1,2,3,4,10,14b-hexahydro-10-methyldibenzo[b,f]pyrido[1,2-d][1,4]diazepin-1-yl)amino]acetate (35 mg, 0.09 mmol) in dioxane (1 mL) was added 4N (aq) NaOH (250 ul). The reaction mixture was stirred at 65° C. for 1.5 h. It was diluted with water (25 mL) whereafter the pH was adjusted to pH 2 with 2N (aq) HCL. The mixture was extracted with ethyl acetate (2×), washed with water and brine, dried (MgSO4) and evaporated. The crude product was purified with LC-MS to afford the title compound (4 mg, 12%). Data (m/z)=372 (M+H)+.
WORKUP
后处理
- extractionThe mixture was extracted with ethyl acetate (2×)
- washwashed with water and brine
- dry with materialdried (MgSO4)
- customevaporated
- customThe crude product was purified with LC-MS