HRID2072378

反应详情

EQUATION

反应方程式

HRID 2072378 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
230 °C

PROCEDURE

实验过程

One hundred forty five grams (1.0 mole) 8-hydroxyquinoline, 40 gm. sodium hydroxide, 500 ml. methanol and 5 gm. potassium iodide were combined in a two liter round bottom flask. To this was added 243 gm. dodecenyl chloride (as used in Example I) and the mixture stirred under reflux overnight. The product was filtered, taken up in ether and washed with 500 ml. Claisen's alkali (in five portions). The ether solution was washed several times with water until neutral, dried and the solvent stripped to yield 317.9 gm. of crude product. Of this amount, 310.9 gm. was distilled through a one foot Vigreaux after being heated in the pot to 230° C. and cooled to about 100° C. The fractions coming off at 197°-202° C., 0.7 mm. Hg. (51.1 gm.) and 202°-231° C., 0.8 mm. Hg. (96.8 gm.) consisted almost entirely of 7-dodecenyl-8-hydroxyquinoline.

WORKUP

后处理

  1. additionTo this was added 243 gm
  2. temperatureunder reflux overnight
  3. filtrationThe product was filtered
  4. washwashed with 500 ml
  5. washThe ether solution was washed several times with water until neutral,
  6. customdried
  7. customto yield 317.9 gm
  8. distillationwas distilled through a one foot Vigreaux
  9. temperaturecooled to about 100° C
  10. customcoming off at 197°-202° C.
  11. custom(51.1 gm.) and 202°-231° C., 0.8 mm. Hg