2-METHYL-4-NITROPHENYL ISOCYANATE synthesis
- Product Name:2-METHYL-4-NITROPHENYL ISOCYANATE
- CAS Number:56309-59-2
- Molecular formula:C8H6N2O3
- Molecular Weight:178.14
Yield:56309-59-2 88%
Reaction Conditions:
in ethyl acetate;toluene at 0 - 100; for 6 h;Heating / reflux;
Steps:
1.1a
2-Methyl-4-nitroaniline (35.0 g, 230 mmol) was dissolved in ethyl acetate (400 ml) and cooled to 0 0C. Phosgene (180 ml, 20% in toluene) was added drop wise over 30 min, precipitation of a white salt followed instantly. After the last addition the temperature was allowed to slowly rise to room temperature, and then the reaction mixture was brought to reflux (about 100 0C). It was refluxed for 2 h 30 min, after which 200 ml of solvent was distilled off before the temperature was lowered to 80 0C and phosgene (140 ml, 20% in toluene) was added drop wise. After the last addition the reaction solution was refluxed for 3 hours, allowed to cool to room temperature and concentrated to dryness. The brown/yellow material was dissolved in diethyl ether (250 ml), filtered and concentrated to give a pale brown powder (36 g, 88 %).
References:
WO2007/64227,2007,A1 Location in patent:Page/Page column 28; 40
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