HRID488977

反应详情

EQUATION

反应方程式

HRID 488977 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

A mixture of 1.0 gram of 7,14-dihydropentacene-5,12-dione and pentacene-5,7(12H,14H)-dione, and 10 mL of 2-methoxyethyl ether was stirred and flushed with nitrogen for 15 minutes. To this was added 1.03 grams of sodium borohydride and stirring was continued at room temperature overnight. To the mixture was added 10 mL of 2-methoxyethyl ether and 6.3 mL of methanol and stirring was continued for 1.5 hours at room temperature. To the mixture was added 15 mL of acetic acid and 10 mL of concentrated hydrochloric acid. The mixture was stirred for one hour at room temperature and heated to 60° C. for one hour. To the mixture was added 50 mL of water, and the resulting solid was isolated by filtration and washed with water. The solid was washed with tetrahydrofuran until a pale filtrate resulted. The solid was washed with heptane and dried to give pentacene.

WORKUP

后处理

  1. customflushed with nitrogen for 15 minutes
  2. additionTo this was added 1.03 grams of sodium borohydride
  3. stirringstirring
  4. additionTo the mixture was added 10 mL of 2-methoxyethyl ether and 6.3 mL of methanol
  5. stirringstirring
  6. waitwas continued for 1.5 hours at room temperature
  7. additionTo the mixture was added 15 mL of acetic acid and 10 mL of concentrated hydrochloric acid
  8. stirringThe mixture was stirred for one hour at room temperature
  9. additionTo the mixture was added 50 mL of water
  10. customthe resulting solid was isolated by filtration
  11. washwashed with water
  12. washThe solid was washed with tetrahydrofuran until a pale filtrate
  13. customresulted
  14. washThe solid was washed with heptane
  15. customdried