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A kind of method for preparing dihydronopol alcohol by hydrogenation reduction of nopol alcohol

A technology for dihydronopol and nopol, which is applied in hydrogenation preparation, chemical instruments and methods, hydroxyl compound preparation, etc., can solve problems such as not giving yield data, and achieve the effect of improving molar yield

Active Publication Date: 2021-07-20
BENGBU CHINA SYNCHEM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] "Journal of the American Chemical Society, 1959, vol.81, p.3440" uses metal platinum as a catalyst to carry out hydrogenation reduction in ethanol, but no yield data is given

Method used

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  • A kind of method for preparing dihydronopol alcohol by hydrogenation reduction of nopol alcohol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] A method for preparing dihydronopol by hydrogenation reduction of Nopol alcohol comprises the steps:

[0031] (1) In a 1L high-pressure hydrogenation kettle, dissolve 200g of Nopol alcohol in 500g of water, add 1g of ruthenium carbon (5wt% ruthenium content) and 1g of Turkish red oil, and heat to 120°C for 6h under a hydrogen atmosphere of 0.2MPa , get the crude product;

[0032] (2) After the crude product was filtered to remove the catalyst, the mixture was allowed to stand for stratification, and the oil and water were separated. The oil phase was dihydronopol, and the molar yield was 97.5%.

[0033] The dihydronopol that obtains is carried out following performance characterization:

[0034] The purity of the obtained dihydronopol (compared with standard substance for qualitative comparison) by gas chromatography (conditions: 10°C / min to 280°C from 80°C) was 97.4%.

Embodiment 2

[0048] The only difference with Example 1 is that the catalyst of step (1) is a mixture of 0.8g ruthenium carbon and 0.96g tetrabutylammonium bromide as catalyst, and the molar yield of dihydronopol is 93.6%.

[0049] The dihydronopol that obtains is carried out following performance characterization:

[0050] Gas chromatography (condition: 10°C / min from 80°C to 280°C) tested the obtained dihydronopol (standard substance comparison qualitative), and the purity was 96.2%.

Embodiment 3

[0052] The only difference with Example 1 is that the catalyst of step (1) is a mixture of 1.2g ruthenium carbon and 0.96g tetrabutylammonium bromide as catalyst, and the molar yield of dihydronopol is 97.1%.

[0053] The dihydronopol that obtains is carried out following performance characterization:

[0054] Gas chromatography (conditions: 10°C / min from 80°C to 280°C) tested the obtained dihydronopol (standard substance comparison qualitative), and the purity was 98.7%.

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Abstract

The invention relates to a method for preparing dihydronopol alcohol by hydrogenation reduction of nopol alcohol, the method comprising the following steps: (1) dissolving nopol alcohol in water, adding ruthenium carbon and turkey red oil, and heating under a hydrogen atmosphere React to obtain the crude product; (2) After the crude product is filtered to remove the catalyst, the mixture is allowed to stand for stratification, and the oil phase is dihydronopol. The method for preparing dihydronopol alcohol by hydrogenation reduction of nopol alcohol provided by the present invention can reduce the number of four-membered ring-opening ring-opening side effects in the chemical structure of nopol alcohol during the hydrogenation reduction process of nopol alcohol by selecting a specific catalyst and phase transfer catalyst. The generation of reaction improves the molar yield (more than 93%) of dihydronopol; Especially when catalyst selection mass ratio is the mixture of Turkish red oil and ruthenium carbon of 0.8~1.2:1, the dihydronopol Molar yield ≥ 97%.

Description

technical field [0001] The invention belongs to the field of intermediate synthesis, and in particular relates to a method for preparing dihydronopol by hydrogenation reduction of nopol. Background technique [0002] Dihydronopol is an important raw material of the drug pinaverium bromide, which is a selective gastrointestinal calcium ion antagonist for the treatment of irritable bowel syndrome. Dihydronopol is obtained by hydrogenating nopol. The disclosed method of preparing dihydronopol by hydrogenation of nopol is as follows: [0003] 1. Document 1: [0004] "Chemical Reagents, 2007, 29 (10), 640" uses palladium carbon as a catalyst, cyclohexene as a hydrogen donor, and toluene as a solvent for reflux for 48 hours to prepare dihydronopol with a molar yield of 86%. This method The hydrogen donor is cyclohexene, which is more expensive than hydrogen reduction. [0005] 2. Document 2: [0006] "Molecules, 2009, vol.14, #8, p.2780-2800" uses platinum oxide as a catalyst...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C29/17C07C31/137
CPCC07C29/172C07C2602/42C07C31/137
Inventor 刘洪强徐剑霄赵士民张浩
Owner BENGBU CHINA SYNCHEM TECH CO LTD