| 摘要 |
#CMT# #/CMT# Preparation of spiro-orthoester comprises reaction of a lactone with an epoxide in the presence of a catalyst such as a heterogeneous acid catalyst; excluding fluorinated sulfonic acid group containing ion exchanger resin. #CMT#USE : #/CMT# The invention deals with the preparation of spiro-orthoester. #CMT#ADVANTAGE : #/CMT# The catalyst is separated after the reaction and is used again. The process is carried out continuously (all claimed). The process is simple and provides the product in high yield. #CMT#INORGANIC CHEMISTRY : #/CMT# Preferred Components: The heterogeneous acid catalyst is ion exchanger resin, tone mineral, zeolite, oxidized carrier material carrying Bronsted acids, alkaline- and alkaline earth metal fluoride, acid metal oxide of the element aluminum (Al), cerium, thorium, titanium (Ti), zirconium, tin (Sn), lead, arsenic, bismuth, antimony, vanadium, chromium (Cr), molybdenum, tungsten, zinc (Zn) or cadmium (Cd), acid metalsulfide of Cd or Zn, sulfate, phosphate and halogenide of the element magnesium, calcium, strontium, barium, copper, Zn, Cd, Al, iron, cobalt, nickel, Cr, potassium, boron, Ti, Sn or silver, oxide mixture or heteropolyacid. Preferred Process: The process is carried out in: a tube reactor with solid bed catalyst or a Wirbelbett-reactor. #CMT#[Image]#/CMT# #CMT#ORGANIC CHEMISTRY : #/CMT# Preferred Components: The lactone is a cyclic ketone compound of formula (I). The epoxide is an oxirane compound of formula (II). The spiro-orthoester is a dioxolane compound of formula (III). The lactone is beta -propiolactone,gamma -butyrolactone, delta -valerolacton, epsilon-caprolactone, cumarin, gamma -decalactone, delta -decalactone or delta -dodecalactone. (II) is ethyleneoxide, propyleneoxide, butyleneoxide, epichlorohydrine, styrolepoxide, glycidylalkylester, butyleneoxide, isobutyleneoxide or vinyloxirane. X : optionally substituted and saturated 2-12C alkylene group, where one or more non-adjacent methyl group is substituted by -O-, -C(O)O-, -C(O)-, -S- or -NR- and two adjacent methyl group is substituted by the carbon atoms of an aromatic aniline; either R1>-R4>, X : 1-18C alkyl, 2-18C alkenyl, phenyl (all optionally substituted), H or -COOR5>; or two residues of R1>-R4>optionally saturated 2-18C alkylene; and R5>1-8C alkyl. #CMT#EXAMPLE : #/CMT# Oxiran-2-carbonic acid methylester (5.27 g) and gamma -butyrolactone (2.22 g) were taken in a gas autoclave, and boro-zeolite (0.53 g) was added. The autoclave was locked and was heated, subsequently under stirring, at 160[deg]C. The reaction mixture was worked up to give 1,4,6-trioxaspiro[4.4]-nonan-2-carbonic acid methylester. |
