反应详情

To 500 ml of CH2Cl2 was added 53 ml (294 mmol) of nonanoyl chloride and 50 g (293.4 mmol) of bis(trimethylsilyl)acetylene. The reaction mixture was cooled in an ice bath and 40 g (300 mmol) of AlCl3 was added portionwise with stirring over 1/2 hour. After stirring for an additional hour the reaction mixture was quenched with ice. Water was added to the reaction mixture and it was extracted 3× with 200 ml aliquots of diethyl ether. The combined extracts were washed 2× with 50 ml aliquots of saturated NaHCO3, 1 × with brine, and then dried (MgSO4). The solvent was removed in vacuo to give a brown oil which was used without further purification.

1. temperatureThe reaction mixture was cooled in an ice bath
2. stirringAfter stirring for an additional hour the reaction mixture
3. customwas quenched with ice
4. additionWater was added to the reaction mixture and it
5. extractionwas extracted 3× with 200 ml aliquots of diethyl ether
6. washThe combined extracts were washed 2× with 50 ml aliquots of saturated NaHCO3, 1 × with brine
7. dry with materialdried (MgSO4)
8. customThe solvent was removed in vacuo
9. customto give a brown oil which
10. customwas used without further purification