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4-Methyl-3-nitropyridine

4-Methyl-3-nitropyridine structure

CAS No:
5832-44-0
Formula:
C6H6N2O2
Chemical Name:
4-Methyl-3-nitropyridine
Synonyms:
Pyridine,4-methyl-3-nitro-;4-Picoline,3-nitro-;4-Methyl-3-nitropyridine;3-Nitro-4-picoline
Categories:
Pharmaceutical Intermediates > Bulk Drug Intermediates

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Description

Deliquescent cryst

4-Methyl-3-nitropyridine Basic Attributes

Molecular Weight：

138.126

Exact Mass：

138.12

DSSTox ID：

DTXSID70334743

HScode：

2933399090

Characteristics

PSA：

58.7

XLogP3：

Appearance：

Deliquescent cryst

Density：

1.2±0.1 g/cm3

Melting Point：

180-182 °C

Boiling Point：

85 °C

Flash Point：

95.9±21.8 °C

Refractive Index：

1.558

Safety Information

Packing level：

Ⅲ

Hazard category：

6.1

Transport codes：

2810

wgk germany：

hazard class code：

6.1

safety instructions：

S26-S39

Marks：

Xn:Harmful

Precautionary statement(s)：

P261-P280-P305 + P351 + P338

Hazard Statements：

H302-H315-H318-H335

GHS Classification：

|Danger|H302 (97.67%): Harmful if swallowed [Warning Acute toxicity, oral]|P261, P264, P270, P271, P280, P301+P312, P302+P352, P304+P340, P305+P351+P338, P310, P312, P321, P330, P332+P313, P337+P313, P362, P403+P233, P405, and P501|Aggregated GHS information provided by 43 companies from 3 notifications to the ECHA C&L Inventory. Each notification may be associated with multiple companies.

4-Methyl-3-nitropyridine Use and Manufacturing

60 g of the dinitrogen pentoxide solid collected in the step 1) of was introduced, and 300 g of sulfur dioxide liquid was introduced at -30 ° C, and the mixture was sufficiently stirred and dissolved to be used. 30g of 4-methylpyridine at -30 under the sulfur dioxide into the liquid 120g, fully dissolved, slowly dropping sulfur dioxide pentoxide solution, the full reaction for 5min, the reaction solution was slowly added to 300g of ice water , Fully hydrolyzed and then adjusted to pH 8-9 by adding sodium carbonate. Add 290g toluene extraction twice combined extract, extract the solvent removed after vacuum distillation 3-nitro-4-methyl pyridine 39g, by gas chromatography detection, purity 99.0percent. (3.642 g, 26.37 mmol; Lancaster) in ethyl acetate (36 mL) was treated with 10% Pd/C (0.25 g) under a hydrogen atmosphere (60 psi) for 30 minutes. The catalyst was removed by filtration and the solution was concentrated to provide the title product as a white solid (2.92 g, 100%). MS (DCI/NH3) m/z 109 (M+H)+.In a 250 ml stainless steel autoclave, Add 13.8 g (0.1 mol) of (13.8 g, 0.1 mol) was dissolved in a methanol solution, and 10% Pd/C (0.1 g) was added. The reaction was carried out in an autoclave, and hydrogen gas was passed to a pressure of 0.5 MPa. , the temperature was raised to 20 C, and the reaction was carried out for 15 h.TLC was monitored until the reaction was complete, cooled to room temperature, diatomaceous earth was filtered, and the filter cake was washed with dichloromethane.This prevented Pd/C from catching fire, and the filtrate was concentrated under reduced pressure to concentrate 2-methyl-4-aminopyridine in a molar yield of 93%.

Computed Properties

Molecular Weight:138.12
XLogP3:1
Hydrogen Bond Acceptor Count:3
Exact Mass:138.042927438
Monoisotopic Mass:138.042927438
Topological Polar Surface Area:58.7
Heavy Atom Count:10
Complexity:132
Covalently-Bonded Unit Count:1
Compound Is Canonicalized:Yes

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4-Methyl-3-nitropyridine

CAS No.: 5832-44-0

Grade: Industrial Grade

Content: 99%

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