HRID1517384
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 methyl 2-((4-methoxy-N,2,6-trimethylphenylsulfonamido)methyl)-1H-benzo[d]imidazole-7-carboxylate (2.40 mmol, 1.0 eq.) was added dropwise to a suspension of LAH (5.28 mmol, 2.2 eq.) in abs. THF (5 ml) under N2 at 0° C. When the addition had ended, the reaction mixture was warmed to room temperature and stirred for 2 h. The reaction mixture was then quenched with THF/water (9:1; 3 ml), while cooling, and filtered over Celite. The filtrate was concentrated to dryness and the crude product was purified by column chromatography over silica gel to obtain the desired product. Yield: 75%
WORKUP
后处理
- customat 0° C
- additionWhen the addition
- customThe reaction mixture was then quenched with THF/water (9:1; 3 ml)
- temperaturewhile cooling
- filtrationfiltered over Celite
- concentrationThe filtrate was concentrated to dryness
- customthe crude product was purified by column chromatography over silica gel