HRID260309

反应详情

EQUATION

反应方程式

HRID 260309 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Allyl 3-nitrophenoxyacetate (5 g, 0.021M) was dissolved in a mixture of ethyl acetate (45 ml) and t-butanol (5 ml), and SnCl2.2H2O (23.79 g, 0.105M) added. After stirring and heating at 60° for 1 hour, sodium borohydride (399 mg, 0.0105M) was added in portions, and heating continued for another 2 hours. Solvent was removed, the residue was taken up in water, and the pH adjusted to 7.6 with aqueous NaHCO3. Organics were extracted into ethyl acetate, and the combined organic layers washed with aqueous NaHCO3, water, brine, and dried (MgSO4). Evaporation gave the title compound (2.61 g).

WORKUP

后处理

  1. additionadded
  2. temperatureheating at 60° for 1 hour
  3. temperatureheating
  4. customSolvent was removed
  5. extractionOrganics were extracted into ethyl acetate
  6. washthe combined organic layers washed with aqueous NaHCO3, water, brine
  7. dry with materialdried (MgSO4)
  8. customEvaporation