CAS RN: 3945-69-5 | Product Number: D2919
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|Purity / Analysis Method||>95.0%(HPLC)|
|Molecular Formula / Molecular Weight||C__1__0H__1__7ClN__4O__3 = 276.72|
|Physical State (20 deg.C)||Solid|
|Store Under Inert Gas||Store under inert gas|
|Condition to Avoid||Hygroscopic,Heat Sensitive|
|Reaxys Registry Number||8026872|
|PubChem Substance ID||87560457|
|Appearance||White to Almost white powder to crystal|
|Purity(HPLC)||min. 95.0 area%|
|Purity(with Total Nitrogen)||min. 98.0 %(calcd.on dried substance)|
|Drying loss||max. 17.0 %|
|Solubility (soluble in)||Methanol|
|Hazard Statements||H302 : Harmful if swallowed.
H314 : Causes severe skin burns and eye damage.
|Precautionary Statements||P260 : Do not breathe dust or mist.
P280 : Wear protective gloves/ protective clothing/ eye protection/ face protection.
P303 + P361 + P353 : IF ON SKIN (or hair): Take off immediately all contaminated clothing. Rinse skin with water.
P301 + P330 + P331 : IF SWALLOWED: Rinse mouth. Do NOT induce vomiting.
P304 + P340 + P310 : IF INHALED: Remove person to fresh air and keep comfortable for breathing. Immediately call a POISON CENTER/doctor.
P305 + P351 + P338 + P310 : IF IN EYES: Rinse cautiously with water for several minutes. Remove contact lenses, if present and easy to do. Continue rinsing. Immediately call a POISON CENTER/doctor.
To a solution of 3-phenylpropionic Acid (1.80 g, 12.0 mmol) and 2-phenylethylamine (1.60 g, 13.2 mmol) in MeOH (120 mL) was added DMTMM (3.65 g, 13.2 mmol) and the mixture was stirred at room temperature for 1 hour. The solvent was removed under reduced pressure. Saturated aqueous sodium bicarbonate solution (100 mL) was added to the residue. After being stirred for 10 minutes, the mixture was extracted with diethyl ether (100 mL). The separated organic layer was washed with deionized water (50 mL), 1 mol/L hydrochloric acid (50 mL), deionized water (50 mL) and brine (100 mL), dried over magnesium sulfate and filtered. The solvent was removed under reduced pressure and the residue was purified by column chromatography (2:1 ethyl acetate / hexane on SiO2), giving white solid (2.54 g, 84%).
The reaction mixture was monitored by TLC (hexane : ethyl acetate = 1 : 1, Rf = 0.30) and GC.
Analytical Data (N-Phenylethyl-3-phenylpropaneamide)
1H NMR (400 MHz, CDCl3); δ 7.05–7.28 (m, 10H), 5.31 (br s, 1H), 3.46 (q, J = 6.8 Hz, 2H), 2.92 (t, J = 7.6 Hz, 2H), 2.71 (t, J = 6.8 Hz, 2H), 2.40 (t, J = 7.6 Hz, 2H).
13C NMR (101 MHz, CDCl3); δ 172.0, 140.8, 138.8, 128.7 (2C), 128.6, 128.5, 128.3, 126.4, 126.2, 40.5, 38.5, 35.6, 31.6.
- Formation of carboxamides by direct condensation of carboxylic acids and amines in alcohols using a new alcohol- and water-soluble condensing agent: DMT-MM
- 4-(4,6-dimethoxy-1,3,5-triazin-2-yl)-4-methyl-morpholinium chloride: an efficient condensing agent leading to the formation of amides and esters
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- 2)Formation of carboxamides by direct condensation of carboxylic acids and amines in alcohols using a new alcohol- and water-soluble condensing agent: DMT-MM
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