반응 #2044991

반응 방정식

tert-butylcyclopentadiene

acetic acid

→

5-tert-butyl-1,1,3-trimethyl-1,2-dihydropentalene

용매

acetone

반응 조건

후처리

1. 1
   workup.ADDITIONIn an ice water bath, 82.1 g (1.15 mol) of pyrolydine was dropwise added
2. 2
   온도under reflux
3. 3
   workup.DISTILLATIONFrom the resulting crude product, the solvent was distilled off under reduced pressure (150 torr, 40° C.)
4. 4
   세척the resulting product was washed with water
5. 5
   건조by drying over magnesium sulfate
6. 6
   workup.DISTILLATIONAfter the solvent was distilled off
7. 7
   workup.DISTILLATIONthe remainder was purified by vacuum distillation, whereby 23.4 g of 5-tert-butyl-1,1,3-trimethyl-1,2-dihydropentalene
8. 8
   기타was obtained
9. 9
   기타The results of the measurement

실험 절차

In a 1000 ml five neck flask, 24.97 g (204 mmol) of tert-butylcyclopentadiene and 399.04 g of acetone were placed. In an ice water bath, 82.1 g (1.15 mol) of pyrolydine was dropwise added, followed by stirring for 18 hours under reflux. In an ice water bath, 70.91 g (1.18 mol) of acetic acid was dropwise added. From the resulting crude product, the solvent was distilled off under reduced pressure (150 torr, 40° C.), and the resulting product was washed with water, a 5% acetic acid solution, a saturated sodium hydrogen carbonate aqueous solution and a saturated saline solution, followed by drying over magnesium sulfate. After the solvent was distilled off, the remainder was purified by vacuum distillation, whereby 23.4 g of 5-tert-butyl-1,1,3-trimethyl-1,2-dihydropentalene represented by the following formula [1] was obtained. Identification was carried out by a 1H-NMR spectrum and a GC-mass spectrometry spectrum (GC-MS). The results of the measurement are given below.

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