HRID368601

反应详情

EQUATION

反应方程式

HRID 368601 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Triethylamine (2.02 g, 20 mmol) was added to a mixture of the compound of Example b (2.47 g, 10 mmol) and N-ethyl-N-(1-methylhept-1-yl)amine (3.15 g, 20 mmol) in toluene (25 mL). The reaction was stirred 2.5 h at ambient temperature, then was partitioned between ethyl acetate and dilute citric acid. The organic phase was washed twice with sat aq NaHCO3, followed with brine, then was dried (MgSO4), concentrated, and kugelrohr distilled under vacuum. The fraction which distilled at 157° C. was collected to afford 1.16 g of the title compound as an amber oil, a 38% yield.

WORKUP

后处理

  1. customwas partitioned between ethyl acetate and dilute citric acid
  2. washThe organic phase was washed twice with sat aq NaHCO3
  3. dry with materialwas dried (MgSO4)
  4. concentrationconcentrated
  5. distillationkugelrohr distilled under vacuum
  6. distillationThe fraction which distilled at 157° C.
  7. customwas collected