公开(公告)号：EP2081682A2

公开(公告)日：2009-07-29

申请号：EP07814783.2

申请日：2007-09-10

申请人： SIGNA CHEMISTRY LLC ,  Lefenfeld, Michael ,  Dye, James L. ,  Nandi, Partha ,  Jackson, James

发明人： LEFENFELD, Michael ,  DYE, James, L. ,  NANDI, Partha ,  JACKSON, James

IPC分类号： B01J23/02 ,  B01J23/04 ,  B01J23/08 ,  B01J23/00 ,  B01J21/00 ,  B01J21/04 ,  B01J20/00

CPC分类号： C07F1/02 ,  C01C1/026 ,  C01D15/00 ,  C01P2002/86 ,  C01P2002/87 ,  C01P2002/89 ,  C01P2006/16 ,  Y02P20/52

摘要： The invention relates to lithium metal/porous metal oxide compositions. These lithium metal compositions are prepared by mixing liquid lithium metal with a porous metal oxide in an inert atmosphere under exothermic conditions sufficient to absorb the liquid lithium metal into the porous metal oxide pores. The lithium metal/porous metal oxide compositions of the invention are preferably loaded with lithium metal up to about 40% by weight, with about 20% to 40% by weight being the most preferred loading. The invention also relates to lithium reagent-porous metal oxide compositions having RLi absorbed into a porous oxide. In formula RLi, R is an alkyl group, an alkenyl group, an alkynyl group, an aryl group, an alkaryl group, or an NR1R2 group; R1 is an alkyl group, an alkenyl group, an alkynyl group, an aryl group, an alkaryl group; and R2 is hydrogen, an alkyl group, an alkenyl group, an alkynyl group, an aryl group, and an alkaryl group. The preparation and use of these compositions are also described.

公开(公告)号：EP1768926A2

公开(公告)日：2007-04-04

申请号：EP05785526.4

申请日：2005-06-14

申请人： SIGNA CHEMISTRY LLC ,  Michigan State University

发明人： LEFENFELD, Michael ,  DYE, James, L.

IPC分类号： C01B25/01

CPC分类号： C11D7/04 ,  C01B3/06 ,  C01B3/08 ,  C01B33/06 ,  C11D17/042 ,  F24V30/00 ,  Y02E60/364

摘要： The invention relates to a method of making alkali metal silicide compositions, and the compositions resulting from the method, comprising mixing an alkali metal with silicon and heating the resulting mixture to a temperature below about 475 °C. The resulting compositions do not react with dry O 2 . Also, the invention relates to sodium silicide compositions having a powder X-ray diffraction pattern comprising at least three peaks with 2Theta angles selected from about 18.2, 28.5, 29.5, 33.7, 41.2, 47.4, and 56.2 and a solid state 23 Na MAS NMR spectra peak at about 18 ppm. Moreover, the invention relates to methods of removing a volatile or flammable substance in a controlled manner. Furthermore, the alkali metal silicide compositions of the invention react with water to produce hydrogen gas.

公开(公告)号：EP2035465A2

公开(公告)日：2009-03-18

申请号：EP07750696.2

申请日：2007-02-13

申请人： SIGNA CHEMISTRY LLC

发明人： LEFENFELD, Michael ,  DYE, James, L. ,  NANDI, Partha ,  JACKSON, James

IPC分类号： C08F2/46

CPC分类号： C07D211/96 ,  C07C209/62 ,  C07C213/08 ,  C07C2601/14 ,  Y02P20/55 ,  C07C211/35 ,  C07C211/40 ,  C07C211/45 ,  C07C217/08

摘要： The invention relates to a method for removing an alkyl sulfonyl or aryl sulfonyl protecting group from a primary or secondary amine by contacting an alkyl sulfonamide or an aryl sulfonamide with a Stage 0 or Stage I alkali metal - silica gel material in the presence of a solid proton source under conditions sufficient to form the corresponding amine. The invention also relates to a method for removing an alkyl sulfonyl or aryl sulfonyl protecting group from a primary or secondary amine by a) reacting an alkyl sulfonamide or an aryl sulfonamide with a Stage 0 or Stage I alkali metal - silica gel material, and b) subsequently reacting the reaction product from step a) with an electrophile or a proton source. Preferred Stage 0 or Stage I alkali metal - silica gel materials include Na, K2Na, and Na2K.

公开(公告)号：EP1807199A2

公开(公告)日：2007-07-18

申请号：EP05800331.0

申请日：2005-09-22

申请人： SIGNA CHEMISTRY LLC ,  Michigan State University

发明人： LEFENFELD, Michael ,  DYE, James, L.

IPC分类号： B01J23/04 ,  C07F1/02 ,  C07C17/25

CPC分类号： C01G23/00 ,  B01J21/04 ,  B01J21/063 ,  B01J23/04 ,  B01J35/1061 ,  B01J35/1066 ,  B01J37/0081 ,  B01J37/0201 ,  B01J37/023 ,  B01J37/08 ,  C01B3/042 ,  C01B3/065 ,  C01B3/08 ,  C01P2006/16 ,  C07C1/26 ,  C07C2/861 ,  C07C5/324 ,  C07C17/23 ,  C07C2521/04 ,  C07C2521/06 ,  C07C2523/04 ,  Y02E60/362 ,  Y02E60/364 ,  C07C15/18 ,  C07C15/20

摘要： The invention relates to Group 1 metal/porous metal oxide compositions comprising porous metal oxide selected from porous titanium oxide and porous alumina and an alkali metal or an alkali metal alloy. The compositions of the inventions are described as Stage 0 and I materials. These materials differ in their preparation and chemical reactivity. Each successive stage may be prepared directly using the methods described below or from an earlier stage material. Stage 0 materials may, for example, be prepared using liquid alloys of Na and K which are rapidly absorbed by porous metal oxide under isothermal conditions, preferably at or just above room temperature, to form loose black powders that retain much of the reducing ability of the parent metals. When the low melting Group 1 metals are absorbed into the porous metal oxide at about 150°C, an exothermic reaction produces Stage I material, loose black powders that are stable in dry air. Further heating forms higher stage materials of unknown composition. It is believed that Stage I higher materials represent reductions of the porous metal oxide after absorption of the Group 1 metal. Preferred Group 1 metal/porous metal oxide compositions of the invention are those containing sodium, potassium, or sodium-potassium alloys with sodium and sodium-potassium alloys being most preferred. Each stage of the Group 1 metal/porous metal oxide composition of the invention may be used as a reducing agent reacting with a number of reducible organic materials in the same manner known for alkali metals and their alloys.

公开(公告)号：EP1692075A2

公开(公告)日：2006-08-23

申请号：EP04811935.8

申请日：2004-11-24

申请人： Lefenfeld, Michael

发明人： LEFENFELD, Michael ,  DYE, James, L.

IPC分类号： C01B3/00

CPC分类号： B01J35/002 ,  B01J20/02 ,  B01J20/103 ,  B01J20/28047 ,  B01J20/28078 ,  B01J20/28097 ,  B01J20/281 ,  B01J20/291 ,  B01J20/3078 ,  B01J20/3204 ,  B01J20/3236 ,  B01J23/04 ,  B01J37/023 ,  B01J37/08 ,  B01J2220/42 ,  B01J2220/54 ,  B01J2220/56 ,  B01J2220/58 ,  C01B3/001 ,  C01B3/06 ,  C07C2/861 ,  C07C2/868 ,  C07D333/76 ,  Y02E60/324 ,  Y02E60/36 ,  C07C15/18 ,  C07C15/14

摘要： The invention relates to Group 1 metal/silica gel compositions comprising silica gel and an alkali metal or an alkali metal alloy. The compositions of the inventions are described as Stage 0, I, II, and III materials. These materials differ in their preparation and chemical reactivity. Each successive stage may be prepared directly using the methods described below or from an earlier stage material. Stage 0 materials may, for example, be prepared using liquid alloys of Na and K which are rapidly absorbed by silica gel (porous Si02) under isothermal conditions, preferably at or just above room temperature, to form loose black powders that retain much of the reducing ability of the parent metals. When the low melting Group 1 metals are absorbed into the silica gel, a mild exothermic reaction produces Stage I material, loose black powders that are indefinitely stable in dry air. Subsequent heating to 400°C produces Stage II materials, which are also loose black powders. Further heating above 400°C forms Stage III material with release of some Group 1 metal. It is believed that Stage I, II and III materials represent reductions of the silica gel after absorption of the Group 1 metal. Preferred Group 1 metal/silica gel compositions of the invention are those containing sodium, potassium, or sodium-potassium alloys with sodium and sodium- potassium alloys being most preferred. Each stage of the Group 1 metal/silica gel composition of the invention may be used as a reducing agent reacting with a number of reducible organic materials in the same manner known for alkali metals and their alloys.