تفاعل #2265
ord-b7fb0104fad94bc0b378012d50f6c0c8
الكواشف
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المعالجة
- 1درجة الحرارةthe reaction mixture was refluxed for 2 hours
- 2أخرىwas bubbled into the mixture
- 3درجة الحرارةAfter cooling
- 4أخرىthe reaction was quenched with saturated ammonium chloride
- 5استخلاصextracted with ether (2×100 ml)
- 6غسيلThe combined ether extracts were washed with brine
- 7تجفيفdried over magnesium sulfate
- 8أخرىevaporated
- 9أخرىto yield the product which
- 10workup.DISTILLATIONwas distilled under high vacuum at 68°-74° C.
- 11أخرىto 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.