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CAS No. :	24078-21-5
Formula :	C₉H₉NO₄
M.W :	195.17
SMILES Code :	C1=C(C(=CC=C1C(OC)=O)[N+](=O)[O-])C
MDL No. :	MFCD00085640
InChI Key :	IEFONJKJLZFGKQ-UHFFFAOYSA-N
Pubchem ID :	260927

GHS Pictogram:
Signal Word:	Warning
Hazard Statements:	H302
Precautionary Statements:	P280-P305+P351+P338

Yield	Reaction Conditions	Operation in experiment
		3-Formyl-4-nitro-benzoic acid methyl ester. A solution of 3-methyl-4-nitro-benzoic acid methyl ester (24.99 g, 128.1 mmol) and N,N-dimethylformamide dimethyl acetal (40.0 mL, 300 mmol) was heated at 1400C for 22.5 h. After cooling to rt, the reaction mixture was concentrated and the residue was crystallized from MeOH to give a purple solid. This solid was dissolved in THF (500 mL) and water (500 mL), and sodium periodate (62.62 g, 292.8 mmol) was added followed by additional sodium periodate (15.6 g, 72.9 mmol) two hours later. After stirring at rt for an additional 1 h, the reaction mixture was filtered through Celite washing with EtOAc (2 L). The filtrate was washed with saturated NaHCO3 (600 mL) and the organic layer was dried over Na2SO4. After filtration, the filtrate was concentrated and the residue was passed through a pad of silica gel, washing with CH2Cl2/hexanes (75percent- 100percent). The filtrate was concentrated and dried to give 3-formyl-4-nitro-benzoic acid methyl ester as yellowish solid. MS (EI): cal'd 210.0 (MH+), exp 210.2 (MH+).
		With a stirrer,A thermometer and a dropping funnel were charged in a 2L three-necked flask35 g of 2,4-dimethylnitrobenzeneAnd 4 g of tetrabutylammonium bromide,And 1000 mL of distilled water was added,Into the water bath,Heated to 90 ,Start the agitator to 300r / min speed stirring;During the stirring,And 85 g of potassium permanganate was added in three portions,After stirring for 1 h,The filtrate was immediately separated by filtration,And the pH was adjusted to 3 with a sulfuric acid solution having a mass concentration of 30percentInto the Buchner funnel,Washed with deionized water and then filtered three times to obtain solid powder; A 2 L three-necked flask equipped with a mechanical stirrer was charged with 70 g of the above separated solid powderAnd 700mL concentration of 40percent methanol solution,Into the water bath,Was heated to 90 20min after dissolution was slowly added dropwise by pipette 50mL concentration of 0.2mol / L sulfuric acid solution,Dropping speed control so that the drop is completed within 30min,Reflux reaction 2h after filtration,Washing and drying to obtain light yellow crystal;50 g of the light yellow crystals obtained above were placed in a stoppered Erlenmeyer flask,10 g of potassium permanganate was added,And then the mixture into the water bath,Heating to 40 degrees Celsius,Stirring with a glass rod for 10 minutes to obtain a mixed liquid;To the above mixture, 20 mL of an acetic acid solution having a mass concentration of 30percent was addedAnd 3 g iron powder,Into the ultrasonic oscillator,Ultrasonic vibration reaction 30min,Ultrasonic power of 100W,Ultrasound frequency of 25KHz,After the end of the ultrasound, the reaction solution was extracted with n-hexane,The organic phase was separated,Into a distillation device,Heated to 85 ° C,After the removal of n-hexane by distillationTo give methyl 3-aldehyde-4-nitrobenzoate.

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CAS No.: 24078-21-5

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CAS No.: 24078-21-5

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[ 24078-21-5 ] Synthesis Path-Downstream 1~3

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Physical hazards
Code	Phrase
H200	Unstable explosive
H201	Explosive; mass explosion hazard
H202	Explosive; severe projection hazard
H203	Explosive; fire, blast or projection hazard
H204	Fire or projection hazard
H205	May mass explode in fire
H220	Extremely flammable gas
H221	Flammable gas
H222	Extremely flammable aerosol
H223	Flammable aerosol
H224	Extremely flammable liquid and vapour
H225	Highly flammable liquid and vapour
H226	Flammable liquid and vapour
H227	Combustible liquid
H228	Flammable solid
H229	Pressurized container: may burst if heated
H230	May react explosively even in the absence of air
H231	May react explosively even in the absence of air at elevated pressure and/or temperature
H240	Heating may cause an explosion
H241	Heating may cause a fire or explosion
H242	Heating may cause a fire
H250	Catches fire spontaneously if exposed to air
H251	Self-heating; may catch fire
H252	Self-heating in large quantities; may catch fire
H260	In contact with water releases flammable gases which may ignite spontaneously
H261	In contact with water releases flammable gas
H270	May cause or intensify fire; oxidizer
H271	May cause fire or explosion; strong oxidizer
H272	May intensify fire; oxidizer
H280	Contains gas under pressure; may explode if heated
H281	Contains refrigerated gas; may cause cryogenic burns or injury
H290	May be corrosive to metals
Health hazards
Code	Phrase
H300	Fatal if swallowed
H301	Toxic if swallowed
H302	Harmful if swallowed
H303	May be harmful if swallowed