HRID1095712

反应详情

EQUATION

反应方程式

HRID 1095712 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Naphthalen-2-ylmethyl carbonochloridate (11.00 g, 49.85 mmol) was dissolved in THF (25 mL) and this was added dropwise to a cooled (0° C.) solution of 1,2,3,6-tetrahydropyridine (3.79 ml, 41.5 mmol) and NaHCO3 (4.18 g, 49.8 mmol) in water (88 mL). A precipitate formed in the reaction immediately, therefore after the addition, additional THF (63 mL) was added to solubilize the reaction mixture. The solution was removed from the bath and warmed to ambient temperature for 16 hours. The reaction was concentrated in vacuo then methylene chloride was added. The mixture was separated, the aqueous layer was washed with methylene chloride, and the combined organics were dried over Na2SO4 and concentrated in vacuo to provide the desired product as an oil (11 g).

WORKUP

后处理

  1. additionthis was added dropwise to
  2. customA precipitate formed in the reaction immediately
  3. additionwas added
  4. customThe solution was removed from the bath
  5. concentrationThe reaction was concentrated in vacuo
  6. additionmethylene chloride was added
  7. customThe mixture was separated
  8. washthe aqueous layer was washed with methylene chloride
  9. dry with materialthe combined organics were dried over Na2SO4
  10. concentrationconcentrated in vacuo