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Wednesday 31 December 2014

Production of 5-hydroxy-7-methoxy-4-methylphthalide in a culture of Penicillium crustosum


figure 3 1H NMR spectrum of 5-hydroxy-7-methoxy-4-methylphthalide (400 MHz, DMSO). 

The 1H NMR spectrum of 5-hydroxy-7-methoxy-4-methylphthalide (Figure 3) showed signals for methyl group at δ 1.95 (H-9, singlet, 3H), a signal for the methoxyl group at δ 3.79 (H-8, singlet, 3H), a signal corresponding to one methylene group at δ 5.15 (H-3, singlet, 2H), and a signal for aromatic hydrogen at δ 6.49 (H-6, singlet, 1H).



Figure 1 Structures of the compounds mycophenolic acid and 5-hydroxy-7-methoxy-4-methylphthalide. 












TABLE I 1H, 13C and gHMBC NMR data for the compounds mycophenolic acid and 5-hydroxy-7methoxy-4methylphthalide 
PositionMycophenolic acid5-hydroxy-7methoxy-4methylphthalide
δ 13Cδ 1H(multiplicity, J in Hz)1H-13C gHMBC*δ 13Cδ 1H(multiplicity, J in Hz)1H-13C gHMBC *
1173.0-173.0--
370.05.18 (2H, br s)1; 3a68.05.15 (2H, br s)1; 3a; 4; 5; 7; 7a
3a122.1--104.0--
4116.7--110.0--
5163.7--163.0--
6106.4--98.06.49 (1H, s)1; 4; 5; 7; 7a
7153.7--158.0--
7a144.0--151.0--
861.03.74 (3H, s)557.03.79 (3H, s)7
911.52.13 (3H, s)3; 3a; 4; 511.01.95 (3H, s)3a; 4; 5
OH-7.67 (1H, br s)--10.59 (1H, br s)4; 6; 5
1’179.1-----
2’32.72.38-2.47 (2H,m)1’; 3’; 4’---
3’34.22.24-2.32 (2H,m)1’; 2’; 4’; 5’; 7’---
4’133.9-----
5’123.05.23-5.28 (1H,m)3’; 7’---
6’22.33.37 (2H, br d; 6.8)5; 7; 5’---
7’16.11.78 (3H, s)3’; 4’; 5’--
Abbreviations: - singlet, br s - broad singlet, br d - broad doublet, - multiplet.










Figure 2 1H NMR spectrum of mycophenolic acid (400 MHz, CDCl3). 
The 1H NMR spectrum of the mycophenolic acid (Figure 2) showed signals for a methyl group at δ 1.78 (H-7', singlet, 3H) and a methyl group linked to aromatic ring at δ 2.13 (H-9, singlet, 3H), a signal for a methoxyl group at δ 3.74 (H-8, singlet, 3H), two signals corresponding to aliphatic methylenes in the region of δ 2.47 to δ 2.38 (H-3a' and H-3b', multiplet 2H), of δ 2.32 to δ 2.24 (H-2', multiplet, 2H), a broad doublet for a methylene group at δ 3.37 (H-6', 2H), a broad singlet at δ 5.18 (H-3, 2H) referring to an aliphatic methylene bearing oxygen, and a multiplet for a methyne group of δ 5.23 to δ 5.28 (H-5',1H).

Figure 4 gHMBC NMR experiment of 5-hydroxy-7-methoxy-4-methylphthalide (400 MHz, DMSO) and important long range correlations detected. 

Anais da Academia Brasileira de Ciências

Print version ISSN 0001-3765

An. Acad. Bras. Ciênc. vol.85 no.2 Rio de Janeiro Apr./June 2013 Epub June 17, 2013

http://dx.doi.org/10.1590/S0001-37652013005000024 


http://www.scielo.br/scielo.php?pid=S0001-37652013000200487&script=sci_arttext











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Tuesday 30 December 2014

Synthesis of 1- (1-adamantyl) -3,4,5-trinitro-1H-pyrazole.

Synthesis of 1- (1-adamantyl) -3,4,5-trinitro-1H-pyrazole.
To 1.5 g (0.00739 mol) of 3,4,5-trinitro-1H-pyrazole in 20 ml of diethyl ether at 0 ° C was added dropwise a solution of 1 g (0.00739 mol) of 1,3-svezhevozognannogo dehydroadamantane in 20 ml of diethyl ether. The mixture was kept under stirring for 1 hour at 0 ° C, the temperature was raised why to reflux and held for an additional 3 hours. The solvent was distilled off. The product was purified by recrystallization from ethanol.






Yield 2.44 g (98%). Mp = 139-140 ° C.
Mass spectrum, m / z (intensity,%): 337 (M + , 2%), 292 ([M-NO 2 ] + , 2%), 247 (2%), 245 ([M- (NO 2 ) 2 ] +, 2%), 199 ([M-3NO 2 ] + , 2%), 177 (36%), 151 (21%), 150 (48%), 135 (Ad + , 96%), 121 (48%), 107 (56%) 95 (71%), 93 (100%) 67 (45%) 55 (75%).
NMR 1 H (300 MHz, DMSO-d 6 ), δ, ppm .: 1.66 (6H, CH 2 , H delta -Ad), with 2.1 (3H, CH, H y -Ad), 2.18 to (6H, CH 2 , H beta -Ad).
NMR 13 C (75.47 MHz, CDCl 3 ), δ, ppm .: 71.8872 (s, 1C, C alpha -Ad), 41.0302 (s, 3C, C beta -Ad), 35.2616 (s, 3C, C delta -Ad), 29.9234 (s, 3C, C y -Ad).

A process for production of 1- (1-adamantyl) -3,4,5-trinitro-1H-pyrazole (RU 2528404):













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5-(hydroxymethyl)-2-furaldehyde




Rf 0.55 (ethyl acetate:hexane = 2:1)

Mp.: 28˚C - 32˚C (lit.: 31˚C - 32˚C [6] ). 

IR νmax (KBr, cm−1): 3405, 3123, 2926, 2851, 1675, 1523, 1397, 
1370, 1334, 1280, 1192, 1023. 

1NMR (800 MHz, DMSO-d6) δH 4.51 (d, 2H, J = 6.0 Hz, CHO); 
5.59 (t, 1H, J = 6.0 Hz, OH); 6.61 (d, 1H, J = 3.5 Hz, H-4); 7.50 (d, 1H, J = 3.5 Hz, H-3); 9.55 (s, 1H, CH=O). 

MS(EI): 126 (C6H6O3). EI-MS (rel. int.%): 126(96); 109(10); 97(100); 81(4); 
69(24); 53(9); 41(50); 39(22).







HPLC spectrum
Machine type: Agilent 1260 Infinity LC
Column: Agilent ZORBAX-C18, 4.6mm×150mm
Mobile phase: methanol:water=5:95(0 min)-100:0(15 min), gradient elution
Flow rate: 1 ml min-1
Measurement temperature: room temperature
Detector: UV, wavelength at 278 nm
Sample concentration: 0.5 g L-1
HMF液相










FT-IR spectrum
Measurement type: BRUKER TENSOR 27
Method: KBr pellet
Sample: 10mg HMF:150mg KBr
Wavelength range: 400-4000cm-1
HMF-IR






1H-NMR spectrum
Machine type: 400MHz AVANCE III
Sample weight: 30mg
Solvents:CDCl3





13C-NMR spectrum
Machine type: 400MHz AVANCE III
Sample weight: 30mg
Solvent: CDCl3
Frequency: 100.6 MHz

五、The main derivatives of HMF:
HMF衍生物_watermark






















Major application fields:
The main application of 5-hydroxymethylfurfual  is as platform chemicals.  Now, HMF  can be  synthesized  fragrance  as a precursor substance.  In addition, HMF can be used in  fine  chemicals   synthesis,  including  pharmaceuticals,  agrochemicals,   macrocycles,  heterocycles,  sugar   derivatives.  In the future,  the main  application  is  to  substitute  oil  to produce  biofuel and  bio-based polymers  as precursor.
...................


Hydroxymethylfurfural
Hydroxymethylfurfural
Identifiers
CAS number67-47-0 Yes
ChemSpider207215 Yes
KEGGC11101 Yes
ChEBICHEBI:412516 Yes
ChEMBLCHEMBL185885 Yes
Jmol-3D imagesImage 1
Properties
Molecular formulaC6H6O3
Molar mass126.11 g/mol
Density1.29 g/cm3
Melting point30 to 34 °C (86 to 93 °F; 303 to 307 K)
Boiling point114 to 116 °C (237 to 241 °F; 387 to 389 K) (1 mbar)
λmax282 nm[1]
Related compounds
Related furan-2-carbaldehydesFurfural
Except where noted otherwise, data are given for materials in their standard state (at 25 °C (77 °F), 100 kPa)



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