Benzoic acid, 5-Methyl-2-[[(1-Methylethoxy)carbonyl]aMino]-4-(trifluoroMethyl)-, Methyl ester synthesis
- Product Name:Benzoic acid, 5-Methyl-2-[[(1-Methylethoxy)carbonyl]aMino]-4-(trifluoroMethyl)-, Methyl ester
- CAS Number:872624-54-9
- Molecular formula:C14H16F3NO4
- Molecular Weight:319.28
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Yield:872624-54-9 99%
Reaction Conditions:
with pyridine in dichloromethane;toluene at 0 - 20; for 2 h;
Steps:
3.5
Step 5; Preparation of methyl 2-(A/-Isopropoxycarbonyl)amino-5-methyl-4-trifluromethylbenzoate; Add isopropyl chloroformate (900 mL, 900 mmol, 1 M in toluene) dropwise to a solutionof methyl 2-amino-5-methyl-4-trifluorornethylbenzoate (200 g, 858 mmol) and pyridine(170 mL, 2.14 mol) in anhydrous dichloromethane (2 L) at 0 - 5 °C under an atmosphereof nitrogen, keeping the internal reaction temperature below 5 °C during the addition.Allow the solution/suspension to warm to room temperature and stir for 2 h. Add 1 MHC1 (2 L) and stir the mixture for 10 min. Collect the organic phase and wash with brine(1 L), dry over anhydrous magnesium sulfate, filter and remove the solvents underreduced pressure at 45 °C to give the title compound as a yellow crystalline solid (283 g,>99%).
References:
WO2006/2342,2006,A1 Location in patent:Page/Page column 57-58
![CarbaMic acid, [2-iodo-4-Methyl-5-(trifluoroMethyl)phenyl]-, 1-Methylethyl ester (9CI)](/CAS/GIF/872624-69-6.gif)