(r)-1-(1-(2-naphthyl) ethyl) thiourea-modified mn-anderson type heteropolyacid catalyst, preparation method and application thereof
A heteropoly acid and catalyst technology, applied in the field of catalytic chemistry, can solve the problems of high dosage, low catalyst activity, and difficult recycling, and achieve high catalytic activity, high enantioselectivity, and environmental friendliness
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0033] Polyacid matrix [N(C 4 H 9 ) 4 ] 4 [α-Mo 8 O 26 ] Preparation
[0034] In a 50mL flask, add Na 2 MoO 4 ·2H 2 O 5.00 g (20.7 mmol) was dissolved in 12 mL of deionized water, and 5.17 mL of 6.0N hydrochloric acid solution was added, and stirred vigorously at room temperature for 1 to 2 minutes. Then, 3.34 g (10.4 mmol) of tetrabutylammonium bromide was dissolved in 10 ml of deionized water and added to the flask under vigorous stirring to immediately form a white precipitate. After the mixture was stirred for 10 minutes, the precipitate was collected in a medium porosity filter and suctioned and washed with 20 mL of water, 20 mL of ethanol, 20 mL of acetone and 20 mL of ether. This crude product (4.78g) was dissolved in 35mL of acetonitrile, and allowed to stand still at -10°C for 24h. The clear, colorless, massive crystals were collected by suction filtration and dried under vacuum for 12 hours. The transparency of the crystal is lost when it is dried. The yield is 3.58 ...
Embodiment 2
[0036] Preparation of (R)-1-(1-(2-naphthyl)ethyl)isothiocyanate
[0037] Add (R)-(+)-1-(2-naphthyl)ethylamine (0.8562g, 5mmol) in a dry reaction vessel, dissolve it with 20mL ethanol, and then slowly add CS 2 (0.1142g, 15mmol) and triethylamine (0.506mg, 5mmol), after stirring the reaction at room temperature for 1h, and then adding di-tert-butyl dicarbonate (Boc 2 O) (1.091mg, 5mmol) and 4-dimethylaminopyridine (DMAP) (18mg, 0.15mmol), after stirring the reaction at room temperature for 2h (gas is generated during the stirring process, attention should be paid to venting and reducing pressure) to obtain 0.8448 g (R)-1-(2-(naphthyl)ethyl)isothiocyanate. The yield was 79.6%.
[0038] The NMR spectrum of (R)-1-(1-(2-naphthyl)ethyl)isothiocyanate is as follows image 3 As shown, the nuclear magnetic data is as follows:
[0039] 1 H NMR(501MHz, CDCl 3 )δ7.94–7.77(m,4H), 7.50(ddd,J=10.0,7.1,1.8Hz,3H), 5.12(d,J=6.8Hz,1H), 1.79(d,J=6.8Hz,3H ).
Embodiment 3
[0041] Preparation of Mn-Anderson type polyoxometalate modified with bilateral amino groups
[0042] Take [N(C 4 H 9 ) 4 ] 4 [α-Mo 8 O 26 ](8.00g,3.7mmol),Mn(CH 3 COO) 3 ·2H 2 O (1.49g, 5.6mmol) and (HOCH 2 ) 3 CNH 2 (1.56g, 12.8mmol), refluxed in 150mL acetonitrile solution for 16h. The orange solution was cooled to room temperature and filtered to remove very fine black solids. The filtrate was exposed to ether vapor. After 2 hours, the white precipitate was filtered off. The orange filtrate was again exposed to ether vapor for several days. A lot of orange crystals were obtained. They are separated by filtration, washed with acetonitrile and a small amount of ether, and dried under vacuum.
[0043] The infrared spectrum of the Mn-Anderson-type polyoxometalate modified with bilateral amino groups is as follows Figure 4 Shown.
[0044] The NMR spectra of Mn-Anderson-type polyoxometalates modified with bilateral amino groups are shown as Figure 5 Shown.
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More - R&D
- Intellectual Property
- Life Sciences
- Materials
- Tech Scout
- Unparalleled Data Quality
- Higher Quality Content
- 60% Fewer Hallucinations
Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.
© 2025 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com