HRID1517384

反应详情

EQUATION

反应方程式

HRID 1517384 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customat 0° C
  2. additionWhen the addition
  3. customThe reaction mixture was then quenched with THF/water (9:1; 3 ml)
  4. temperaturewhile cooling
  5. filtrationfiltered over Celite
  6. concentrationThe filtrate was concentrated to dryness
  7. customthe crude product was purified by column chromatography over silica gel