HRID1414936

反应详情

EQUATION

反应方程式

HRID 1414936 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

Allow 5 -m-methoxyphenylpent-1-yne (8 g.) to stand for 12 hours at 70° C under nitrogen with water (2.5 cc), trioxan (0.5 g), 30% formalin (5.5 g), diethylamine (4 g), acetic acid (2.75 g), dioxan (25 cc) and cuprous chloride (0.13 g). Make the cooled solution alkaline with 10% aqueous sodium hydroxide and extract with ether; then extract the ether extract with 10% hydrochloric acid: wash the acid extract with ether, make alkaline with 10% aqueous sodium hydroxide, extract with ether, and then wash and dry the ether extract. Distil to obtain 1-diethylamino-6-m-methoxyphenylhex-2-yne (10.6 g. 88%), b.p. 130°-131° C/0.1 mm.

WORKUP

后处理

  1. extractionextract with ether
  2. extractionthen extract the ether
  3. extractionextract with 10% hydrochloric acid
  4. washwash the acid
  5. extractionextract with ether
  6. extractionextract with ether
  7. washwash
  8. dry with materialdry the ether
  9. extractionextract
  10. customDistil