Dodec-11-yn-1-ol (CAS # 18202-10-3)
Dodec-11-yn-1-ol (CAS # 18202-10-3)
kev npaj | NaH (7.5g, 60% roj dispersion, 326mmol) tau ntxiv batch los ntawm batch rau dodecyl -3-alkyne -1-cawv (10.0g,54.95mmol; GF Smith) nyob rau hauv ib tug stirred 0 ℃ tov ntawm ethylenediamine (40mL). Tom qab 1 teev, qhov kub tau nce mus rau 70 ℃. Tom qab lwm 8h, txias cov tshuaj tiv thaiv sib tov rau 0 ° C, ua tib zoo txiav nrog dej txias (100mL), thiab rho tawm nrog ether (3 × 60mL). Qhov sib xyaw ether extract tau ntxuav nrog dej (100mL). Cov dej ntxuav tau rov qab rho tawm nrog ether (3 × 60mL). Kev sib xyaw ua ke cov organic extracts tau concentrated nyob rau hauv lub tshuab nqus tsev, thiab cov residues raug rau kab chromatography siv 10% EtOAc / hexane kom tau 11-dodecyne -1-cawv (7.4g, 74%) kis nrog 3-5% ntawm lwm lub cheeb tsam isomers ( regioisomer). 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). |
Sau koj cov lus ntawm no thiab xa tuaj rau peb