HRID614003

反应详情

EQUATION

反应方程式

HRID 614003 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

55.75 grams of ethylchlorocarbonate in 100 cc of anhydrous benzene are gradually added at 5° C. to a stirred solution of 81 grams of 2,3-dihydro-6-methoxy-2-methyl-4-benzofuranamine and 46 cc of triethylamine in 700 cc of anhydrous benzene. At the end of the addition, the reaction mixture is slightly warmed and stirring is continued, at room temperature, for 3 hours. After this time the reaction mixture is refluxed for two hours, then cooled, washed with water, dried over Na2SO4 and concentrated to dryness yielding 95.81 grams (83.5 percent of theoretical) of the compound of the title B.p./0.4 mmHg 172° C.

WORKUP

后处理

  1. additionAt the end of the addition
  2. temperaturethe reaction mixture is slightly warmed
  3. temperatureAfter this time the reaction mixture is refluxed for two hours
  4. temperaturecooled
  5. washwashed with water
  6. dry with materialdried over Na2SO4
  7. concentrationconcentrated to dryness
  8. customyielding 95.81 grams (83.5 percent of theoretical) of the compound of the title B.p
  9. custom0.4 mmHg 172° C.