反应详情

To a stirred solution of 14.4 g. of valeryl chloride and 20.4 g. of bis-trimethylsilylacetylene in 300 ml. of dry methylene chloride, cooled in an ice bath, is added powdered anhydrous aluminum chloride, portionwise, over a period of 20 minutes. The mixture is stirred for 5 minutes, then the cooling bath is removed and the mixture is stirred at room temperature for 4 l hours. The mixture is poured into 500 ml. of ice-water. The organic layer is separated, washed with water and brine, dried over anhydrous sodium sulfate and filtered through diatomaceous earth. The mother liquor is evaporated to dryness giving a brownish residue. This residue is Kugelrohr-distilled to give 16.56 g. of colorless liquid at 45° C./0.3 mm which is essentially identical with the authentic product.

1. additionis added
2. customthe cooling bath is removed
3. stirringthe mixture is stirred at room temperature for 4 l hours
4. additionThe mixture is poured into 500 ml
5. customThe organic layer is separated
6. washwashed with water and brine
7. dry with materialdried over anhydrous sodium sulfate
8. filtrationfiltered through diatomaceous earth
9. customThe mother liquor is evaporated to dryness
10. customgiving a brownish residue
11. distillationThis residue is Kugelrohr-distilled
12. customto give 16.56 g
13. customat 45° C.