HRID2192556

反应详情

EQUATION

反应方程式

HRID 2192556 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 3-nitro-4-(1,4-dioxaspiro[4.5]dec-7-en-8-yl)pyridine (1.0 equiv.) in 20% TFA in CH2Cl2 (0.2 M) was stirred at room temperature overnight. The solvents were removed under reduced pressure. The residue was dissolved with ethyl acetate (200 mL), and washed with sat NaHCO3 (30 mL), and sat NaCl (30 mL). The organic was dried with MgSO4, filtered and concentrated to give 4-(3-nitropyridin-4-yl)cyclohex-3-enone (85%). The crude product was used to next step without further purification. LC/MS (m/z): MH+=218.9, Rt=0.60

WORKUP

后处理

  1. customThe solvents were removed under reduced pressure
  2. dissolutionThe residue was dissolved with ethyl acetate (200 mL)
  3. washwashed
  4. dry with materialThe organic was dried with MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated