Reaction equation
[C:1]1([CH3:8])[C:2]([CH3:7])=[CH:3][CH:4]=C[CH:6]=1.[OH2:9].[C:10]([OH:13])(=[O:12])[CH3:11].[CH3:14][OH:15]>>[O:9]1[CH2:4][CH2:3][CH:2]([C:14]([OH:12])=[O:15])[CH2:1][CH2:6]1.[CH3:14][O:9][CH2:6][CH2:1][CH:2]1[CH2:7][O:13][C:10](=[O:12])[CH2:11]1.[OH:9][CH2:6][CH2:1][CH:2]1[CH2:7][O:13][C:10](=[O:12])[CH2:11]1.[C:10]([O:13][CH2:4][CH2:3][CH:2]1[CH2:7][O:15][C:8](=[O:9])[CH2:1]1)(=[O:12])[CH3:11]Participants
Procedure
100 parts of bottom product (7) from the first column (1) are passed into the second column (2) with 40 theoretical plates. 0.1 l of xylene (isomer mixture) is added as water entrainer and is returned (10) via line 8 and a phase separator (3) continuously into the column. With a distillate temperature of 28° C., a distillate pressure of 70 mbar and a reflux ratio of 1.6, 23 parts of overhead product (9) of the composition 80.1% by weight of water, 11.2% by weight of acetic acid, 3.3% by weight of methanol, 1.8% by weight of ester of tetrahydropyran-4-carboxylic acid and 44 parts of bottom product (12) with the composition 0.1% by weight of ester of tetrahydropyran-4-carboxylic acid, 10.7% by weight of 3-spirocyclopropylbutyrolactone, 28.9% by weight of 3-(2-methoxyethyl)butyrolactone, 6.1% by weight of 3-(2-hydroxyethyl)butyrolactone and 15.1% by weight of 3-(2-acetoxyethyl)butyrolactone are obtained. At 108° C., 33 parts of side stream (11) with the composition 99.5% by weight of ester of tetrahydropyran-4-carboxylic acid are removed at plate 27.
Sources & evidence
- ORD record
- ord-6d5fb5ec88a04b0cbeaba1bc9c75d4a5
- Source dataset
- uspto-grants-1995_05
- Patent number
- US05414097
Linked notes
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