HRID1823662

反应详情

EQUATION

反应方程式

HRID 1823662 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a one-liter four-necked flask were added 102.5 g (595 mmol) of ethyl (R,R)-2-hydroxycyclohexanecarboxylate and 400 mL of 2-propanol and stirring was started. Hydrazine monohydrate (44.7 g; 893 mmol) was dropped thereinto at 13° C. taking 30 minutes. After the dropping, the mixture was stirred at 80° C. for 9.5 hours. Followed by, heating was stopped and the mixture was cooled to room temperature to precipitate the crystals. The crystals were filtered and washed with a small amount of 2-propanol. The resulting crystals were dried to give 30.10 g of the title compound. The yield was 32%.

WORKUP

后处理

  1. stirringAfter the dropping, the mixture was stirred at 80° C. for 9.5 hours
  2. temperatureFollowed by, heating
  3. customto precipitate the crystals
  4. filtrationThe crystals were filtered
  5. washwashed with a small amount of 2-propanol
  6. customThe resulting crystals were dried