HRID1072403

反应详情

EQUATION

反应方程式

HRID 1072403 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

1-Butanol, 3 methyl, acetate. Under an atmosphere of argon, acetyl chloride (6.5 ml, 91.8 mmol) was added dropwise to a 0° C. solution of isoamyl alcohol (5 ml, 45.9 mmol), N, N-dimethylpyridine (2.8 g, 23 mmol), and anhydrous pyridine (4.1 ml, 50.5 mol) in dichloromethane (92 ml). The reaction mixture was poured into 100 ml of 0.1 N HCl, and the resulting layers were separated. The organic layer was washed with 50 ml of saturated aqueous ammonium chloride then dried over magnesium sulfate. The organic layer was filtered and concentrated in vacuo to a clear oil. The resulting oil was purified by distillation (bp 134-136° C.) to give isoamyl acetate. 1H NMR (300 MHz, CDCl3) 4.08 (t, 2H, J 6.9), 2.03 (s, 3H), 1.68 (m, 1H), 1.51 (q, 2H, J 6.9), 0.92 (d, 6H, J 6.6).

WORKUP

后处理

  1. customthe resulting layers were separated
  2. washThe organic layer was washed with 50 ml of saturated aqueous ammonium chloride
  3. dry with materialthen dried over magnesium sulfate
  4. filtrationThe organic layer was filtered
  5. concentrationconcentrated in vacuo to a clear oil
  6. distillationThe resulting oil was purified by distillation (bp 134-136° C.)