I cacboxilic va cac clorua axit vo co.
UI, KETLUAN.
Nhu vay, biing phuong piiap dnng vong i,3.4-thiadiazol va i,3,4-triazol thdng (lua d/in xuA'l thiosemicacbazit, cbiing tdi da tdng hgp dugc mdi day cdc di^n'^xun't Ihiosemicacbazil, 2-amino-1.3,4-thiadiazol va 1.2-diamino-l.3,4-triazol. Cdc san pham lim dugc da dugc do die^m chay, xac djnh cac gin ni R, vdi he dung mdi phu hgp (bang 2), xac dinh cA'u Ink ihdng qua phd hdng ngoai, Iir iinnai, phd khdi lugng va phd cdng huctng tir hat nhdn 'H-. '-^C NMR. ddng thdi thu hoat tinh khang khuAn vd khang ndm cua mot sd chAi
ItJng hg|i dtrgc (bang I).
I V . T H V C N G H l f i M :
Axit 2-furoic (I!) vd 5-brom-2 fiiioic (111) duac dieu che' Iheo 16]. cac dAn xuAt thiosemicacbazit (Va,b) dugc di^u che ihco |2,3.41.
1. Dieu che 2-amino-5-ffnrvl-2)-1,3.4-lhiadiayol va
2-amino-5-f5-biom- furvl-2)-1.3.4-lhiadlazol (chat Via. VIb)
Nhd giot 2ml H.SO^ dac vao 1.4 g dan xuat thiosemicacbazit. Dun each thuy hdn hgp trong vdng hai tie'ng d nhiet do 50-60"C. Dan xuA't thiosemicacbazit (chat V) hi ciiay ddn ra. Sau khi dun xong. cho san phAm thu dugc vao nudc. Trung hoa dung dich bAng amoniAc de'n mdi irudng kiem (vira trung hoa vira lam lanh). Tiong qua trinh trung hoa. ket tua man vang dugc tach la, lgc lA'y ket tua nay.
Y = H: Dem hoa tan ket tua v;io etyl axetat (cd mot phdn nhd lugng chAi khdng tan). Can lay ph;1n tan ra dem quay cat lhu duoc tinh the mau vang sang dang bdt tan tcM tan). Can lay ph;1n tan ra dem quay cat lhu duoc tinh the mau vang sang dang bdt tan tcM lrong cdn ndng, metanol, ciyl axetat. khd inn (rong clorofonn, tan tdl trong nudc ndng.
Y = Br : Sau khi lgc hiJl ke't liia dcni ket tinh iai lAn nua lir cdn.Tinh the' ihu duoc cn
mdu xam , khd tan trong nudc, etyl axelal, tan tdl Iiong cdn ndng. 2. Dieu che 1.2-diamino-5-(fuivl-2)-1.3,4-tria/ol va 1,2-diamino
•5-(5-brom-rurvl-2)-l.3.4-tmyol (chat Vila. Vllb)
Dun hdi luu hdn hgp gdm I g thiadiazol hoac dan xuA't brom cua nd (chai Via hoac
VIb) vdi 4 ml hidrazin hidrat va 5 ml cdn diing lam dung mdi. Sau dd quay cdt hdn hap d6
loai cdn va hidrazin hidrat du.
Triazol thu dugc cd mau vang sang. linli lli6 huih tru, khd tan trong etyl axetat, tan tdl trong cdn ndng.
Ghi chu: Cong trinh ndy duac hodn thdnh voi sU ho tra kinh phi cua chKony^ trinh khoa hoc ccrhd/i.
TAI LHlU THAM KHAO
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141 Xiao-Wensun. Yanzhang. Indian }. Chem, 38B,l<)99,998-999
|5) U.V.Laddc, S.R. Dcsai, Y.S. Soninnnavat, R.S. Bmnut &S.C. Bcnnnt, Indian J. Chem, 37B,1998,46I-467.
(6) A.A.Ponomarcp. xintczir i icactsi furanovic vrsextv. Izdat. Xaratopxkovc univexitet I960.tr 71.78.