2-(methoxymethyl)aniline synthesis
- Product Name:2-(methoxymethyl)aniline
- CAS Number:62723-78-8
- Molecular formula:C8H11NO
- Molecular Weight:137.18
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Yield:62723-78-8 98.4%
Reaction Conditions:
with palladium 10% on activated carbon;hydrogen in methanol;lithium hydroxide monohydrate at 55 - 70; under 9000.9 Torr;Sealed tube;Pressure;Temperature;Reagent/catalyst;
Steps:
2 Preparation of o-aminobenzyl methyl ether
At room temperature, to 1 L reaction vessel was added 140.0 g 0.833 mol o-nitrobenzyl methyl ether, 600 ml of methanol, 5.0 g of a 10% Pd / C (water content 69%), sealed, nitrogen purging 3 times, hydrogen purging three times, the residual oxygen was measured, when the amount of residual oxygen was <0.2%, the reaction was pressurized with hydrogen to 1.2MPa, the reaction temperature was controlled at 55 to 70 ° C, when the pressure was constant, the reaction was continued with heating for 0.5 h, HPLC was used to monitor the reaction, when the starting material was <0.5%, the reaction was stopped, then cooled to room temperature, the catalyst was recovered by filtration, the solvent was recovered under reduced pressure to give 112.3 g of o-aminobenzyl methyl ether in a yield of 98.4% and HPLC of 98.0%.
References:
CN104744272,2016,B Location in patent:Paragraph 0079; 0080
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