HRID3658

反应详情

EQUATION

反应方程式

HRID 3658 的结构方程式

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

Dissolve 1,2,3,4-tetrahydronaphthalene-2-carboxylic acid (2-amino-4,6-dioxo-3,5-dipropylcyclohex-1-enyl)amide (2.0 g, 5.2 mmol) in ethanol (50 ml), add 15% potassium hydroxide (50 ml) and heat to 70° C. for 4 hours. After cooling to 0° C., acidify the reaction with concentrated hydrochloric acid (13 ml). Add water (100 ml) and collect the resulting precipitate by suction filtration. Purify the white solid by flash chromatography (50% ethyl acetate/hexane) and triturate with 5% diethyl ether/hexane to provide, after drying under vacuum at 120° C. for 30 minutes the title compound (1.04 g), m.p. 202°-204° C.

WORKUP

后处理

  1. temperatureAfter cooling to 0° C.
  2. customAdd water (100 ml) and collect the resulting precipitate
  3. filtrationby suction filtration
  4. customPurify the white solid by flash chromatography (50% ethyl acetate/hexane)
  5. customtriturate with 5% diethyl ether/hexane
  6. customto provide
  7. dry with materialafter drying under vacuum at 120° C. for 30 minutes the title compound (1.04 g), m.p. 202°-204° C.