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With hydrogen;copper chromite; at 60 - 150℃; under 31789.8 Torr;Purification / work up;
Example 1 A crude product stream from a production of 1,4-butanediol carried out in accordance with WO 97/43242 was treated according to the process of the present invention at a reaction temperature of 600C and a pressure of 600 psig, a gas rate of lOOnlph and a LHSV of lhr1 over the catalyst PG85/1. The peak acetal content of the crude feed as measured by the Peak Acetal Test was 0.429wt% and that of the product was found to be 0.234wt%, indicating a 50% removal.; Example 2The reaction of Example 1 was repeated at a temperature of 7O0C. The peak acetal content of the crude feed as measured by the Peak Acetal Test was 0.429wt% and that of the product was found to be 0.212 wt%.; Example 3The reaction of Example 1 was repeated at gas rate of 25nlph. The peak acetal content of the crude feed as measured by the Peak Acetal Test was 0.429wt% and that of the product was found to be 0.252wt%.; Examples 4 to 11A 50ml bed of copper chromite catalyst PG85/1 was activated by the following procedure. The gas rate was set to give the required gas velocity in the reactor and the pressure was set to 50 psig. The gas flow was established using N2 and while the reactor was at room temperature the following procedure was commenced: the H2 concentration was increased to 0.1% and the inlet temperature was brought up to 1200C over 3 hours; the H2 was monitored at the inlet and outlet above 100C and the H2 inlet was kept at 0.1%; during the following steps it was ensured that the exotherm did not exceed 10C by reducing the H2 inlet composition if necessary and the conditions were held until the exotherm reduced; the temperature was then increased by 100C until it reached 16O0C; when at 1600C the H2 in the exit gas only differed slightly from the inlet composition; after being held for 1 hour the inlet gas H2 composition was increased to 0.2% over 1 hour and held for 2 hours; the H2 in the inlet was then increased to 0.3% for 1 hour and held for 2 hours; the H2 in the inlet was then increased to 0.4% for 1 hour and held for 2 hours; the H2 in the inlet was then increased to 0.5% and held until the H2 at the inlet equalled the H2 at the exit; the 0.5% H2 in the inlet was then maintained and the temperature increased to 1700C over 1 hour and it was ensured that the exotherm did not exceed 100C and held until H2 at the inlet equalled the H2 at the exit; the temperature was then maintained at 1700C; the H2 content at the inlet was then slowly increased to 1% over a minimum time of 1 hour and maintained until H2 at the inlet equalled the H2 at the exit; the exotherm was then monitored to keep it below 100C, by reducing H2 concentration if needed, then the H2 concentration was increased up to 5% at 1% per hour; the H2 at the inlet was increased slowly to 10% and maintained until H2 at the inlet equalled the H2 at the exit; the exotherm was monitored to keep it below 100C; the H2 at the inlet was increased to 100% while making sure the exotherm did not exceed 100C; the operating pressure was then increased and left under H2 for 4 hours before the liquid feed was turned on. EPO <DP n="10"/>A crude hydrogenation product containing 0.48wt% of <strong>[64001-06-5]2-(4-hydroxybutoxy)-tetrahydrofuran</strong> precursors Lambdavas passed over the heated reaction zone under the conditions set out in Table 1.Table 1 Example 12A further example demonstrated the present invention on a miniplant scale. A 250ml bed of copper chromite catalyst PG85/1 was activated by the method described above. The reaction conditions are set out in Table 2.Table 2 The crude hydrogenation product had a Peak Acetal of 0.46wt% following treatment this resulted in a level of 19%. The material from this miniplant was distilled via the conventional EPO <DP n="11"/>distillation processes to provide 1 ,4-butanediol product that contained 0.8% 2-(4- hydiOxybutoxy)-tetrahydiOforan. This demonstrated that a high purity polymer grade 1 ,4- butanediol can be achieved in high yield.
4
[ 64001-06-5 ]
[ 76702-30-2 ]
Yield
Reaction Conditions
Operation in experiment
17%
Example 5 10 g of a mixture of <strong>[64001-06-5]2-(4-hydroxybutoxy)tetrahydrofuran</strong> of the formula IIc (83%) and 1,4-bis(2-tetrahydrofuranyloxy)butane (17%) obtained as described in section (b) of Example 1 were hydrogenated at 100 C. and 150 bar in the presence of 1 g of a palladium catalyst (10% of Pd on activated carbon) for 10 hours.
With toluene-4-sulfonic acid; In diethyl ether; at 28℃; for 1.5h;
In eggplant-shaped flask in 2-butanol 14.8g (0.2mmol, manufactured by Wako Pure Chemical Industries, Ltd.), MDHP23.6g (0.24mmol), diethyl ether 150ml (Wako Pure Chemical Industries, Ltd. take Kogyo Co., Ltd.), and stirred at 28 C..Here, p-toluenesulfonic acid monohydrate 0.76 g (4.0 mmol, manufactured by Wako Pure Chemical Industries, Ltd.) was added, and stirring was continued for 1.5 hours and cooled to room temperature.The reaction yield of protecting body A-2 was 97.6%.Once with saturated aqueous sodium carbonate solution 110ml, 3 times with distilled water 110ml, and washed once with saturated brine 110ml.The organic layer was concentrated to give an oily substance 36.6g.The yield protected compound A-2 after the water washing treatment was 97.0%, the recovery rate of the protective body A-2 in the washing process was 98.0%.
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