HRID1259385

反应详情

EQUATION

反应方程式

HRID 1259385 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
-50 °C

PROCEDURE

实验过程

A stirred solution of 7-(2-fluoro-4-trimethylsilanyl-phenylamino)-6-methyl-8-nitro-2,3-dihydro-oxazolo[3,2-a]pyridin-5-one (0.25 g, 0.66 mmol) in dry DCM (10 mL) and iodine monochloride (0.8 mL) were added to silver tetrafluoroborate (0.4 g, 2.05 mmol) in DCM (10 mL) previously degassed with nitrogen for 30 minutes at −50° C. The resulting mixture was stirred at −50° C. for 1 hour. The reaction was monitored by TLC (50% ethylacetate in hexane). This was followed by the addition of 20 mL of sodium thiosulphate and filtered through celite. The filtrate was concentrated to afford 0.2 g of the product (70% yield).

WORKUP

后处理

  1. custompreviously degassed with nitrogen for 30 minutes at −50° C
  2. additionThis was followed by the addition of 20 mL of sodium thiosulphate
  3. filtrationfiltered through celite
  4. concentrationThe filtrate was concentrated