تفاعل #2265

ord-b7fb0104fad94bc0b378012d50f6c0c8

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةthe reaction mixture was refluxed for 2 hours
  2. 2
    أخرىwas bubbled into the mixture
  3. 3
    درجة الحرارةAfter cooling
  4. 4
    أخرىthe reaction was quenched with saturated ammonium chloride
  5. 5
    استخلاصextracted with ether (2×100 ml)
  6. 6
    غسيلThe combined ether extracts were washed with brine
  7. 7
    تجفيفdried over magnesium sulfate
  8. 8
    أخرىevaporated
  9. 9
    أخرىto yield the product which
  10. 10
    workup.DISTILLATIONwas distilled under high vacuum at 68°-74° C.
  11. 11
    أخرىto yield 6.4 g as a colorless liquid

الإجراء التجريبي

To a solution of ethyl magesium bromide (prepared from 2.5 g of magnesium turning and 11.3 g of bromoethane) in ether was added dropwise a solution of 10.2 g of cyclohexylacetylene in ether and the reaction mixture was refluxed for 2 hours. The reaction mixture was cooled to ambient temperature and anhydrous formaldehyde (prepared from the thermal decomposition of 50 g of paraformaldehyde for 20 minutes) was bubbled into the mixture. After cooling, the reaction was quenched with saturated ammonium chloride and extracted with ether (2×100 ml). The combined ether extracts were washed with brine, dried over magnesium sulfate and evaporated to yield the product which was distilled under high vacuum at 68°-74° C. to yield 6.4 g as a colorless liquid.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05728715uspto-grants-1998_03