HRID631996

反应详情

EQUATION

反应方程式

HRID 631996 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

m-CPBA (CAN 937-14-4, 5.0 g, 29.2 mmol) was added to a solution of 5-methyl-pyridine-2-carboxylic acid (CAN 4434-13-3, 2.0 g, 14.6 mmol) in methylene chloride (50 mL) and the mixture was stirred overnight at room temperature. The solid was filtered off, quenched with a saturated solution of sodium thiosulfate (50 mL), and the mixture was extracted with methylene chloride (3×60 mL). The organic layers were combined, dried over anhydrous sodium sulfate and concentrated in vacuo to give yellow solid which was washed with ether (5×20 mL) to give the product (0.9 g, 40.3%); MS (EI): m/e=154.1 [M+H]+.

WORKUP

后处理

  1. filtrationThe solid was filtered off
  2. customquenched with a saturated solution of sodium thiosulfate (50 mL)
  3. extractionthe mixture was extracted with methylene chloride (3×60 mL)
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated in vacuo
  6. customto give yellow solid which
  7. washwas washed with ether (5×20 mL)