HRID420709

反应详情

EQUATION

反应方程式

HRID 420709 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of methyl 6-chloro-5-methyl-3-pyridinecarboxylate (84 mg, 0.453 mmol) in DCM (2 ml), DIBAL-H (1.5 M solution in toluene, 0.905 ml, 1.358 mmol) was added dropwise under N2 at −78° C. The reaction mixture was allowed to attain rt and stirred overnight. After 18 h, TLC showed no starting material. The reaction was quenched by addition of sodium-potassium tartrate saturated solution, extracted with DCM, dried, filtered, and concentrated to afford (6-chloro-5-methyl-3-pyridinyl)methanol (63 mg, 0.400 mmol, 88% yield) pure enough to be used in the next step.

WORKUP

后处理

  1. customto attain rt
  2. waitAfter 18 h
  3. customThe reaction was quenched by addition of sodium-potassium tartrate saturated solution
  4. extractionextracted with DCM
  5. customdried
  6. filtrationfiltered
  7. concentrationconcentrated