Ethyl 4-nitrobenzoate NMR

Ethyl 4-nitrobenzoate

• CAS Number 99-77-4
   

13 C NMR

1H NMR












IR









Ms











INTRODUCTION OF AMINO GROUP

 ethyl-p-aminobenzoate.



Shift (ppm)
167.4 114.1
151.5 60.6
132.0 14.7
120.0





picked up from a japanese site

₉H₁₁NO₂)の¹H-NMRスペクト ル (300MHz)である。図アを示す化合物はIRスペクトル (neat)にて1700 cm^-1付近に、又、図イを示す化合物はIRスペクトル (Nujol)にて 1650 cm^-1付近に共に強い吸収を示す。スペクトルと化合物の正し い組合せはどれか。ただし、図アの3.4 ppm付近、図イの6.3 ppm付近及び7.9 ppm付近のシグナルは重水処理すると消失する。また測定溶媒に基づくシグナ ルは除いてある。

　a　2-ethoxybenzamide
　b　4-ethoxybenzamide
　c　ethyl 3-aminobenzoate
　d　ethyl 4-aminobenzoate

　　　 ア　イ　
　　1　a　c　
　　2　a　d　
　　3　b　c
　　4　b　d　
　　5　c　a　
　　6　c　b

is (a and a) the figure below (C any compound that is shown in a ~ D ₉ H ₁₁ NO ₂ of) ¹ H-NMR spectrum is (300MHz). 1700 cm IR spectrum at (neat) compounds exhibit a Zua ^-1 in the vicinity, also, compounds that exhibit a spinal is 1650 cm IR spectrum at (Nujol) ^-1 shows a strong absorption both in the vicinity. Right combination of compounds and any spectrum. However, I lost signal around 3.4 ppm of Zua, of around 7.9 ppm and 6.3 ppm near the spinal when you heavy water processing. The signal based on the measurement solvent have been removed. 　a 2-Ethoxybenzamide 　b 4-Ethoxybenzamide 　c ethyl 3-Aminobenzoate 　D ethyl 4-Aminobenzoate

　　　 Eye　
　　1 a c　
　　2 a D　
　　b 3 c
　　4 b D　
　　c 5 a　
　　6 c b

THANE INDIA


































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TERIFLUNOMIDE SPECTRAL DATA

Teriflunomide,
HMR-1726, 1726, A-771726, RS-61980, SU-0020,
(Z)-2-Cyano-3-hydroxy-N-[4-(trifluoromethyl)phenyl]-2-butenamide
108605-62-5, 282716-73-8 (monosodium salt)
C12-H9-F3-N2-O2 270.2091

SPECTROSCOPY DATA ]

 ^! HNMR (DMSO, 300MHz) :δ 2.24(s, 3H); 5.36(bs, IH); 7.65(d, J=8.7Hz, 2H);

7.76(d, J=8.6Hz, 2H); 10.89(s, IH) ppm. 

¹³ CNMR (DMSO, 75MHz) :δ 23.5, 82.1, 118.3, 122.2, 126.5, 126.9, 142.1, 167.4,

187.8 ppm.

MS(FD) : m/e 269(M", 100).

 IR : 3305, 2220, 1633, 1596, 1554, 1418, 1405, 1325, 1247, 1114, 1157, 1073, 971,

842, 684 cm-¹.

REF EP 2280938 A2





UPDATED

TERIFLUNOMIDE SPECTRAL DATA

Teriflunomide,
HMR-1726, 1726, A-771726, RS-61980, SU-0020,
(Z)-2-Cyano-3-hydroxy-N-[4-(trifluoromethyl)phenyl]-2-butenamide
108605-62-5, 282716-73-8 (monosodium salt)
C12-H9-F3-N2-O2 270.2091

SPECTROSCOPY DATA

nmr……….http://www.medkoo.com/Product-Data/Teriflunomide/QCData-Teriflunomide-BBC20130720-web.pdf

http://file.selleckchem.com/downloads/nmr/S416901-Teriflunomide-HNMR-Selleck.pdf

17= US2011/0105795A1

1H NMR AND 13C NMR

above 13C NMR

! HNMR (DMSO, 300MHz) :δ 2.24(s, 3H); 5.36(bs, IH); 7.65(d, J=8.7Hz, 2H);

7.76(d, J=8.6Hz, 2H); 10.89(s, IH) ppm.

13 CNMR (DMSO, 75MHz) :δ 23.5, 82.1, 118.3, 122.2, 126.5, 126.9, 142.1, 167.4,

187.8 ppm.

MS(FD) : m/e 269(M”, 100).

 IR : 3305, 2220, 1633, 1596, 1554, 1418, 1405, 1325, 1247, 1114, 1157, 1073, 971,

842, 684 cm-1.

REF EP 2280938 A2

Example-1  Preparation of Ethyl-2-cyano-3-hydroxy-but-2-enoate (III) [77] Potassium carbonate (73.3 g) was added to the well stirred solution of Ethylcy- anoacetate (50 g) in Dimethylformamide (250 ml) and stirred for 15 minute at ambient temperature. Acetic anhydride (90.25 g) was added drop wise to the above well stirred solution during 2 to 3 hours at ambient temperature. Reaction mixture was stirred at ambient temperature for 15 to 20 hours. Reaction mixture was diluted with water (500 ml) and extracted with dichloromethane (3 xlOO ml). Combined organic layer was washed with saturated sodium carbonate solution (3x100ml). Aqueous carbonate layer was separated and acidified with 50% HCl solution and extracted with dichloromethane (3x100ml). Combined organic layer was washed with brine solution (100 ml), dried over sodium sulfate and evaporated to yield Ethyl 2-cyano-3-hydroxy-but-2-enoate (58 g).

Yield: 84.6% Example-2 Preparation of Teriflunomide (I) [82] Ethyl 2-cyano-3-hydroxybut-2-enoate (III) (50 g) and 4-(trifluoromethyl) aniline (51.9 g) in xylene (1000 ml) was refluxed for 48 hours. The reaction mixture was allowed to cool at room temperature. Separated solid was filtered and washed with xylene (2×100 ml). Solid was dried under vacuum at 700C to yield (62 g) of Teri- flunomide.

Yield: 71.0%

Purity: 99.4%

! HNMR (DMSO, 300MHz) :δ 2.24(s, 3H); 5.36(bs, IH); 7.65(d, J=8.7Hz, 2H);

7.76(d, J=8.6Hz, 2H); 10.89(s, IH) ppm.

13 CNMR (DMSO, 75MHz) :δ 23.5, 82.1, 118.3,

122.2, 126.5,

126.9, 142.1, 167.4,

187.8 ppm.

MS(FD) : m/e 269(M”, 100).

IR : 3305, 2220, 1633, 1596, 1554, 1418, 1405, 1325, 1247, 1114, 1157, 1073, 971,

842, 684 cm-1.

1H NMR PREDICT

COSY

HPLC

HPLC method of analysis:

N-(4′-trifluoromethylphenyI)-5-methylisoxazole-4-carboxamide of formula-2:

Apparatus: A liquid chromatographic system equipped with variable wavelength UV- detector; Column: Cosmicsil APT CI 8, 100 x 4.6 mm, 3 μιη (or) equivalent; Flow rate: 1.5 ml/min; Wavelength: 210 nm; Column Temperature: 25°C; Injection volume: 20 μί; Run time: 40 min; Diluent: Mobile phase; Needle wash: Tetrahydrofuran; Elution: Isocratic; Mobile phase: 5 ml of triethyl amine into a 650 ml of water. Adjusted the pH to 3.4 with dil. Orthophosphoric acid and filter this solution through 0.22 μπι nylon membrane filter paper and sonicate to degas it. (Z)-2-cyano-3-hydroxy-but-2-enoicacid-(4-trifluoromethyl phenyl)-amide compound of formula- 1:

Apparatus: A liquid chromatographic system equipped with variable wavelength UV- detector; Column: Kromasil 100 C18, 250 x 4.6 mm, 5 μηι (or) equivalent; Flow rate: 1.0 ml/min; Wavelength: 250 nm; Column Temperature: 35°C; Injection volume: 5 μί; Run time: 37 min; Diluent: 0.01 M dipotassium hydrogen orthophosphate in 1000 ml of water; Elution: Gradient; Mobile phase-A: Buffer (100%); Mobile phase-B: Acetonitrile : Buffer (70:30 v/v); Buffer: 1 ml of ortho phosphoric acid into a 1000 ml of water and 3.0 grams of 1 -octane sulfonic acid sodium salt anhydrous. Adjust pH to 6.0 with potassium hydroxide solution and filtered through 0.22μηι Nylon membrane filter paper and sonicate to degas it……..http://www.google.com/patents/WO2015029063A2?cl=en

WO2009147624A2*	3 Jun 2009	10 Dec 2009	Alembic Limited	A process for preparing teriflunomide
WO2011004282A2*	22 Jun 2010	13 Jan 2011	Alembic Limited	Novel polymorphic form of teriflunomide salts
US5494911	24 Oct 1990	27 Feb 1996	Hoechst Aktiengesellschaft	Isoxazole-4-carboxamides and hydroxyalkylidenecyanoacetamides, pharmaceuticals containing these compounds and their use
US5679709	7 Jun 1995	21 Oct 1997	Hoechst Aktiengesellschaft	N-(4-trifluoromethylphenyl)-2-cyano-3-hydroxycrotonamide or salts, used for reduction of b-cell produced self-antibodies
US5990141	6 Jan 1995	23 Nov 1999	Sugen Inc.	Administering 5-methyl-isoxazole-4-carboxylic acid-n-(4-trifluoromethyl)anilide or 2-cyano-3-hydroxy-n-(4-trifluoro-methyl)phenyl-2-butenamide; antitumor,-carcinogenic and proliferative agents; kinase inhibitors

P.S. : The views expressed are my personal and in no-way suggest the views of the professional body or the company that I represent.

P.S. : The views expressed are my personal and in no-way suggest the views of the professional body or the company that I represent.

P.S. : The views expressed are my personal and in no-way suggest the views of the professional body or the company that I represent.

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COCK SAYS MOM CAN TEACH YOU NMR

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