HRID383780

反应详情

EQUATION

反应方程式

HRID 383780 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
135 °C

PROCEDURE

实验过程

A solution of 7a (160 mg, 0.300 mmol) and hydrazine hydrate (286 μL, 9.18 mmol) in ethanol:toluene (2.70 mL of an 8:1 mixture, respectively) was heated to 100° C. in a sealed microwave vial for 10 min, An additional aliquot of hydrazine hydrate (200 μL, 6.42 mmol) was added, and the resulting mixture was heated to 135° C. in a sealed microwave vial for 15 min. The reaction mixture was cooled to rt and partitioned between EtOAc and water. The combined organics were washed with water and brine, dried (sodium sulfate) and concentrated in vacuo to afford the title compound 9a. m/z (ES) 523 (MH)+.

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled to rt
  2. custompartitioned between EtOAc and water
  3. washThe combined organics were washed with water and brine
  4. dry with materialdried (sodium sulfate)
  5. concentrationconcentrated in vacuo