Dodec-11-yn-1-ol (CAS# 18202-10-3)
Dodec-11-yn-1-ol (CAS# 18202-10-3) Ulwazi
ukulungiselela | I-NaH (7.5g, 60% yokusasazwa kweoli, i-326mmol) yongezwa ibhetshi ngebhetshi kwi-dodecyl -3-alkyne -1-alcohol (10.0g, 54.95mmol; GF Smith) kwisisombululo se-0 ℃ se-ethylenediamine (40mL). Emva kwe-1h, ubushushu bonyuswa ukuya kuma-70 ℃. Emva kwenye i-8h, pholisa umxube wokuphendula kwi-0 ° C, uphelise ngokucophelela ngamanzi abandayo e-ice (100mL), kwaye ukhuphe nge-ether (3 × 60mL). I-extract ether edibeneyo ihlanjwe ngamanzi (100mL). Ukuhlamba amanzi kwakhutshwa ngasemva nge-ether (3 × 60mL). I-extracts ye-organic edibeneyo yayigxininiswe phantsi kwe-vacuum, kwaye i-residus yaphantsi kwekholomu ye-chromatography isebenzisa i-10% ye-EtOAc/hexane ukufumana i-11-dodecyne -1-alcohol (7.4g,74%) engcoliswe nge-3-5% yezinye i-isomers zengingqi ( iregioisomer). TLC:30% EtOAc/hexane, Rf ≈ 0.4;1H NMR(300MHz,CDCl3)δ3.66(t,2H,J = 7.3Hz), 2.14-2.21(m,2H),1.93(t,J = 1.9Hz) ,1H),1.20-1.63(m,16H). |
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