HRID1485292

反应详情

EQUATION

反应方程式

HRID 1485292 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 4-methyl-3-oxopentanenitrile (15 g, 135 mmol) in EtOH (150 mL) was added hydrazine hydrate (7.30 g, 146 mmol) slowly at 0° C. The reaction mixture was heated to reflux for 4 h. Removal of EtOH under reduced pressure gave an oily residue that was dissolved in EtOAc (200 mL) and washed with freshly prepared brine (2×50 mL). The organic layer was dried over anhydrous sodium sulfate. Removal of EtOAc gave 5-isopropyl-1H-pyrazol-3-amine, Compound (ii) (10 g, 59% yield). 1H NMR (400 MHz, CDCl3) δ (ppm): 1.22 (d, 6H), 2.80-2.92 (m, 1H), 4.80 (brs, 3H), 5.41 (s, 1H).

WORKUP

后处理

  1. temperatureThe reaction mixture was heated
  2. temperatureto reflux for 4 h
  3. customRemoval of EtOH under reduced pressure
  4. customgave an oily residue that
  5. washwashed with freshly prepared brine (2×50 mL)
  6. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  7. customRemoval of EtOAc