in tetrahydrofuran T=-60°C; temp. change, introduction of pentanone-3 at different moments; further temp., solvent, reagent; Product distributionMechanism;
参考文献
Mallet, M.; Queguiner, G.
Tetrahedron, 1982 , vol. 38, # 20 p. 3035 - 3042
in tetrahydrofuran under N2, addn. of Li-compound in THF to a soln. of ethyl acetate and CuI in THF (-78°C), stirred (10 min); not isolated;
参考文献
Yoneda, Ryuji; Harusawa, Shinya; Kurihara, Takushi
Journal of the Chemical Society, Perkin Transactions 1: Organic and Bio-Organic Chemistry (1972-1999), 1988 , p. 3163 - 3168
in hexane; cyclohexane to soln. of 1-iodoheptane (1.0 mmol) and TMTH (1.0 mmol) in hexane at 0°C added LDA (1.0 mmol, 1.6 M soln. in cyclohexane) under Ar, react. time 10 min; analyzed by GLPC;
in hexane; cyclohexane to 1-iodoheptane (1 mmol) and TMTH (1 mmol) in hexane at 0°C added LDA (1 mmol, in cyclohexane) under Ar, stirred for 20 min, quenched; analyzed by GLPC;
in diethyl ether; cyclohexane 1-chloroheptane (1 equiv.) and TMTH (2 equiv.) in Et2O cooled to 0°C under Ar, LDA (1 equiv., 1.6 M soln. in cyclohexane) dropped in, stirred for 20-25 min at room temp., quenched with water; analyzed by GC;
water in tetrahydrofuran inert atmosphere; addn. of LDA in THF at -78°C to soln. of Fe-complex; reaction for 1 h; addn. of phosphate; reaction for 1 h; mixt. raised to room temp.; addn. of LDA in THF at -78°C; warmed to room temp.; hydrolysis at 0°C;; extn. of organic layer with CH2Cl2; dried over MgSO4; evapn.; purifn. of oil by flash chromy. (pentane-ether 2:1); crystn. of first yellow fraction (0°C, pentane); elem. anal.;
参考文献
Doisneau, G.; Balavoine, G.; Fillebeen-Khan, T.
Journal of Organometallic Chemistry, 1992 , vol. 425, # 1-2 p. 113 - 117
hydrogenchloride; carbon dioxide in tetrahydrofuran
参考文献
Cai, Sui Xiong; Zhang, Han-Zhong; Drewe, John A.; Reddy, P. Sanjeeva; Kasibhatla, Shailaja; Kuemmerle, Jared Daniel; Ollis, Kristin P.
Patent: US2003/45546 A1, 2003 ;
US 20030045546 A1
