HRID2202597

反应详情

EQUATION

反应方程式

HRID 2202597 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 8.144 g of (R)-3-benzhydryloxypyrrolidine synthesized in Production Example 168, 7.701 g of a known compound ethyl 6-chloromethylpyridine-2-carboxylate, 69 mL of acetonitrile, and 9.0 mL of triethylamine was heated under reflux for 3 hours. After being allowed to cool down, the mixture was diluted with ethyl acetate. The diluted mixture was poured into a saturated saline solution, and the organic layer was collected by separation. The organic layer was washed with a saturated saline solution and dried over magnesium sulfate. The solvent was distilled off, and then the residue was purified by silica gel column chromatography (chloroform/acetone (volume ratio)=15:1 to 10:1) to give the title compound (7.22 g (54%)).

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureunder reflux for 3 hours
  3. temperatureto cool down
  4. additionThe diluted mixture was poured into a saturated saline solution
  5. customthe organic layer was collected by separation
  6. washThe organic layer was washed with a saturated saline solution
  7. dry with materialdried over magnesium sulfate
  8. distillationThe solvent was distilled off
  9. customthe residue was purified by silica gel column chromatography (chloroform/acetone (volume ratio)=15:1 to 10:1)