magnesium in tetrahydrofuran; toluene addn. of 50mmol F2C6H3Br in 20ml THF to 50mmol Mg-filings in 50ml THF at -20°C; warming to room temp. after 4h; stirring for 14h; dropwise addn. of the mixture to 17mmol BCl3*OMe2 in 70ml toluene at -20°C; warming to room temp. after 4h;; removal of solvent; refluxing with n-hexane for 4h; removal of Mg-salts by filtration; crystn. from the filtrate; recrystn. from n-hexane; detn. by (13)C-, (19)F-, (1)H-NMR, m.p., mass spectroscopy;;
参考文献
Naumann, D.; Butler, H.; Gnann, R.
Zeitschrift fuer Anorganische und Allgemeine Chemie, 1992 , vol. 618, p. 74 - 76
Song, Yong-Qi; Yuzuri, Tomoaki; Suezawa, Hiroko; Sakakibara, Kazuhisa; Hirota, Minoru; Nakada, Masahiro
Bulletin of the Chemical Society of Japan, 1997 , vol. 70, # 8 p. 1875 - 1878
Song, Yong-Qi; Yuzuri, Tomoaki; Suezawa, Hiroko; Sakakibara, Kazuhisa; Hirota, Minoru; Nakada, Masahiro
Bulletin of the Chemical Society of Japan, 1997 , vol. 70, # 8 p. 1875 - 1878