Invention Grant
- Patent Title: Purification of esters of tetrahydro-pyran-4-carboxylic acid
- Patent Title (中): 四氢 - 吡喃-4-羧酸酯的纯化
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Application No.: US185179Application Date: 1994-01-24
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Publication No.: US5414097APublication Date: 1995-05-09
- Inventor: Rolf Fischer , Norbert Goetz , Thomas Kuekenhoehner , Harald Rust , Werner Schnurr
- Applicant: Rolf Fischer , Norbert Goetz , Thomas Kuekenhoehner , Harald Rust , Werner Schnurr
- Applicant Address: DEX Ludwigshafen
- Assignee: BASF Aktiengesellschaft
- Current Assignee: BASF Aktiengesellschaft
- Current Assignee Address: DEX Ludwigshafen
- Priority: DEX4141221.4 19911213
- Main IPC: C07D309/08
- IPC: C07D309/08
Abstract:
A process for purifying esters of tetrahydropyran-4-carboxylic acid of the formula I ##STR1## where R.sup.1 to R.sup.3 are each C.sub.1 -C.sub.4 -alkyl, and R.sup.2 and R.sup.3 are each additionally hydrogen, from mixtures produced in the reaction of butyrolactones of the formula II ##STR2## where R.sup.2 and R.sup.3 have the abovementioned meanings, and R.sup.4 is hydrogen, alkyl of 1-6 carbons or acyl of the formula --CO--R.sup.2, with alcohols of the formula R.sup.1 OH in the presence of oxide catalysts, by distillation, which entailsa) removing overhead, in a first column with 5-25 theoretical plates with a distillate pressure of 700-1100 mbar and a distillate temperature of 50.degree.-80.degree. C., an alcohol and up to 10% of the water,b) transferring the bottom product from the first column into a second column with 18-40 theoretical plates, into which a water entrainer is metered between plates 15 and 30, and is circulated, and which operates with a distillate pressure of 35-350 mbar and a distillate temperature of 18.degree.-70.degree. C., with the esters of tetrahydropyran-4-carboxylic acid being removed between plates 8 and 18 at 90.degree.-150.degree. C., and, where appropriate,c) feeding the bottom product from the second column into a third column with 5-25 theoretical plates, and returning the overhead products at a distillate pressure of 1-100 mbar and a distillate temperature of 90.degree.-140.degree. C. to the synthesis of the esters of tetrahydropyran-4-carboxylic acid.
Public/Granted literature
- US4993030A File system for a plurality of storage classes Public/Granted day:1991-02-12
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