HRID638883

反应详情

EQUATION

反应方程式

HRID 638883 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
23 °C

PROCEDURE

实验过程

To a round bottomed flask was loaded 4.2 grams of 2-acetylcyclohexanone, 3.52 grams of (5-Amino-1H-[1,2,4]triazol-3-yl)-methanol and 50 ml 2-methoxyethanol. The mixture was refluxed for 18 hours. Then it was cooled down to 23° C. and concentrated to 5 ml. Then 50 ml ethyl ether was added and the precipitate was filtered and vacuum dried to yielded 3.32 grams of product Yield. 49%. This compound was used directly for the next step. MS: 219.2 (M+H). H-NMR (DMSO): δ 5.49 (t, 1H, OH, J=6 Hz), 4.61 (d, 2H, J=6 Hz), 3.24 (m, 2H), 2.93 (m, 2H), 2.69 (s, 3H), 2.52 (s, 2H), 1.84 (m, 4H).

WORKUP

后处理

  1. customTo a round bottomed flask was loaded
  2. temperatureThe mixture was refluxed for 18 hours
  3. concentrationconcentrated to 5 ml
  4. additionThen 50 ml ethyl ether was added
  5. filtrationthe precipitate was filtered
  6. customvacuum dried