HRID1772173

反应详情

EQUATION

反应方程式

HRID 1772173 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 6-methoxynaphthalene-2-carbonitrile (1.0 g, 5.5 mmol), N-iodosuccinimide (1.4 g, 6.0 mmol) in ACN (10 ml) and TFA (125 μl) is stirred at RT for 4 h. A saturated aqueous solution of sodium hydrogencarbonate is added and the mixture extracted with DCM. The combined organic layers are extracted with an aqueous solution of sodium thiosulfate, dried over MgSO4 and concentrated in vacuo. The product is purified by RP HPLC. Yield: 1.68 g (99%). HPLC-MS: tR=1.32 min (METHOD—1).

WORKUP

后处理

  1. extractionthe mixture extracted with DCM
  2. extractionThe combined organic layers are extracted with an aqueous solution of sodium thiosulfate
  3. dry with materialdried over MgSO4
  4. concentrationconcentrated in vacuo
  5. customThe product is purified by RP HPLC