in diethyl ether freshly prepared, moist AgN3 covered with water cooled to 0°C; addn. of soln. of I2 in ether cooled to 0°C under shaking;; decanting etheric layer at low temp. very fast through dry folder filter into flask with calcined Na2SO4; drying 5 min.; evapn. of ether with dry air until pptn., then in desiccator; washing with small amt. of petroleum ether; (drying); impurity: I2;;
in further solvent(s) addn. of CsN3 in SO2ClF to (ICNI)AsF6 in SO2ClF, stirring (30 min); filtration, the byproducts being identified by gas-phase IR when the filtrate wa carefully evapd. to dryness;
参考文献
Klapoetke, Thomas M.
Journal of the Chemical Society - Dalton Transactions, 1997 , # 4 p. 553 - 557
Hantzsch, A.; Schuemann, M.
Ber., 1900 , vol. 33, p. 522 - 522
Full Text Show Details
Hantzsch, A.; Schuemann, M.
Ber., 1900 , vol. 33, p. 525 - 525
Full Text Show Details
Gmelin Handbook: I: MVol.2, 159, page 600 - 602
in tetrachloromethane
dropwise addn. of Pb2(C6H5)6 in CCl4 to stirred soln. of IN3 in CCl4 over a period of 15 min at -10°C; stirring at -10°C for 1 h; allowing to reach room temp.;; filtration; fractional crystn. on cooling; repeated recrystn.; m.p.; IR spectroscopy;;
Hantzsch, A.; Schuemann, M.
Ber., 1900 , vol. 33, p. 522 - 522
Full Text Show Details
Hantzsch, A.; Schuemann, M.
Ber., 1900 , vol. 33, p. 525 - 525
Full Text Show Details
Gmelin Handbook: I: MVol.2, 159, page 600 - 602