1,1'-二乙酰基二茂铁合成路线 (共 15 条)
反应条件
aluminium chloride in dichloromethane ferrocene (1.0 equiv.) added to a stirred suspension of acetyl chloride (2.2 equiv.) and aluminium chloride (2.2 equiv.) in dichloromethane, stirred at room temp. overnight (16 h); washed with water, organic layer passed through a plug of alumina, washed with chloroform, washings concentrated in vacuo, crude product purified by flash column chromy. on silica gel (TLC Rf 0.24 (1:3 acetone-hexane)), elem. anal.;
参考文献
Carroll, Michael A.; White, Andrew J.P.; Widdowson, David A.; Williams, David J.
Journal of the Chemical Society, Perkin Transactions 1, 2000 , # 10 p. 1551 - 1557
反应条件
aluminium trichloride; acetyl chloride in dichloromethane to a mixt. of AlCl3 and acetyl chloride in dry CH2Cl2 was slowly addedwith stirring and in a stream of N2 a soln. of ferrocene in CH2Cl2; stirred for 2 h and poured in ice, aq. phase sepd. and extd. several timesby CHCl3; extact mixed with the organic phase, evapd., cooled., sublimed in vac. at 120°C;
参考文献
Tomassetti, M.; Curini, R.; D'Ascenzo, G.; Ortaggi, G.
Thermochimica Acta, 1981 , vol. 48, p. 333 - 342
反应条件
acetyl chloride; aluminium trichloride in dichloromethane byproducts: tributyltin chloride; addn. of acetyl chloride to a suspn. of finely powdered AlCl3 in CH2Cl2 at room temp., react. for 10-15 min (forming of CH3COCl*AlCl3 complex), addn. of Fe-complex in CH2Cl2 (-70°C), stirring at -70°C for 10 min; ice water, extn. of aq. phase with CH2Cl2, drying (MgSO4), evapn., distn. at 80°C, 0.08 mmHg, 2 h (isoln. of byproducts), chromy. (SiO2, hexane, CH2Cl2), chromy. of material that not distill (SiO2, 19:1 hexane-ethyl acetate); elem. anal.;
参考文献
Journal of the American Chemical Society, , vol. 113, # 13 p. 4864 - 4870
反应条件
aluminium trichloride in carbon disulfide
参考文献
Doklady Akademii Nauk SSSR, , vol. 106/111, p. 675 - 677
Doklady Akademii Nauk SSSR, , vol. 111, p. 362 - 364
Fe: Org.Verb.A1, 2.5.7.6.5, page 156 - 161
反应条件
aluminium trichloride; acetyl chloride in dichloromethane Friedel-Crafts acylation;;
参考文献
Journal of Organic Chemistry, , vol. 28, p. 1549 - 1554
反应条件
aluminium trichloride in dichloromethane byproducts: (C5H5)Fe(C5H3(COMe)2); (N2); AlCl3 is added to mixt. of iron-complex and acetyl chloride in CH2Cl2 at -42°C, stirring for 75 min; mixt. is poured into ice water, aq. phase is extd. with CH2Cl2, combined extracts are dried (Na2SO4) and concd., chromy. (SiO2, hexane/EtOAc);
参考文献
Organometallics, , vol. 13, p. 2480 - 2485
反应条件
1-ethyl-3-methylimidazolium iodide-AlCl3 (argon); very slow addn. of AlCl3 to 1-ethyl-3-methylimidazolium iodide, addn. of ferrocene to the ionic liquid, stirring (10 min), ice bath (0°C), addn. of AcCl, stirring (0°C, 2 h), quenching (2 M HCl); extraction (CH2Cl2), drying (MgSO4), concn. (vac.), column chromy. (SiO2, hexanes/ethyl acetate, 10:1 to 1:1);
参考文献
Journal of the Chemical Society - Dalton Transactions, , # 1 p. 63 - 66
反应条件
1-ethyl-3-methylimidazolium iodide-AlCl3 (argon); addn. of ferrocene to the ionic liquid 1-ethyl-3-methylimidazolium iodide-AlCl3, stirring (10 min), ice bath (0°C), addn. of Ac2O, stirring (0°C, 2 h), quenching (2 M HCl); extraction (CH2Cl2), drying (MgSO4), concn. (vac.), column chromy. (SiO2, hexanes/ethyl acetate, 10:1 to 1:1);
参考文献
Journal of the Chemical Society - Dalton Transactions, , # 1 p. 63 - 66
反应条件
sodium tetrahydroborate in dichloromethane; trifluoroacetic acid B-compd. addn. to stirred Fe-complex soln., mixt. stirring at 25°C for 1 h, diln. (CH2Cl2), quenching in aq. NaOH, org. layer sepn., drying over Na2SO4, solvent removal; residue flash chromy. (SiO2, Et2O/hexanes 1:9);
参考文献
Bhattacharyya, Sukanta
Journal of the Chemical Society - Perkin Transactions 1, 1996 , # 12 p. 1381 - 1383
反应条件
ammonia; zinc(II) chloride in tetrahydrofuran; diethyl ether; water stirring (room temp., 10 h), Et2O and NH3(aq) addn.; extg. (Et2O), drying (Na2SO4), evapn., chromy. (SiO2, hexanes / Et2O = 9: 1);
参考文献
Bhattacharyya, Sukanta
Organometallics, 1996 , vol. 15, # 3 p. 1065 - 1066