HRID255306

反应详情

EQUATION

反应方程式

HRID 255306 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of tert-butyl {1-[2-(7-fluoro-2-oxoquinoxalin-1(2H)-yl)ethyl]piperidin-4-yl}carbamate (Intermediate 141, 240 mg, 0.62 mmol) in dichloromethane (20 mL) was treated with trifluoroacetic acid (15 mL). After 45 minutes, the reaction was concentrated to dryness, the residue taken up in methanol/chloroform (15:85, 30 mL) and washed with saturated sodium bicarbonate solution. The aqueous layer was re-extracted with methanol/chloroform (15:85, 3×30 mL. The combined organic phases were dried over magnesium sulfate and concentrated to dryness to give 170 mg (quantitative) of the crude product as an oil.

WORKUP

后处理

  1. concentrationthe reaction was concentrated to dryness
  2. washwashed with saturated sodium bicarbonate solution
  3. extractionThe aqueous layer was re-extracted with methanol/chloroform (15:85, 3×30 mL
  4. dry with materialThe combined organic phases were dried over magnesium sulfate
  5. concentrationconcentrated to dryness