Alternatived Products of [ 894351-65-6 ]
Product Details of [ 894351-65-6 ]
| CAS No. : | 894351-65-6 |
MDL No. : | |
| Formula : |
C9H8BrNO4
|
Boiling Point : |
- |
| Linear Structure Formula : | - |
InChI Key : | - |
| M.W : |
274.07
|
Pubchem ID : | - |
| Synonyms : |
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Safety of [ 894351-65-6 ]
| Signal Word: | |
Class: | |
| Precautionary Statements: | |
UN#: | |
| Hazard Statements: | |
Packing Group: | |
Application In Synthesis of [ 894351-65-6 ]
* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
- Downstream synthetic route of [ 894351-65-6 ]
- 1
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[ 99548-54-6 ]
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[ 885519-05-1 ]
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[ 894351-65-6 ]
| Yield | Reaction Conditions | Operation in experiment |
|
With sulfuric acid; nitric acid; at -30 - 10℃; for 0.5h; |
EXAMPLE 128A Methyl 4'-amino-2-methyl-5-nitro-1,1'-biphenyl-3-carboxylate Example 1A (20 g, 87.3 mmol) was cooled to -5 C. and treated dropwise with H2SO4 (100 mL) at such a rate as to maintain the internal temperature below 10 C. The reaction mixture was cooled to -30 C. and treated dropwise with nitric acid (5.7 mL, 91.7 mmol) at such a rate as to maintain the internal temperature below -12 C. After the addition was complete the reaction flask was placed in an ice bath for 30 minutes and poured onto crushed ice. The resulting suspension was extracted twice with diethyl ether and the combined extracts were washed with aqueous NaHCO3 and brine, dried (MgSO4), filtered, and concentrated to give 23 g of a mixture of methyl 3-bromo-2-methyl-5-nitrobenzoate and methyl 3-bromo-2-methyl-6-nitrobenzoate. Substitution of this mixture for Example 1C in Example 1D followed by purification by silica gel chromatography with 10 to 40% ethyl acetate/hexanes provided the desired product. 1H NMR (300 MHz, DMSO-d6) delta 2.46 (s, 3H), 3.91 (s, 3H), 5.36 (s, 2H), 6.67 (d, J=8.5 Hz, 2H), 7.07 (d, J=8.1 Hz, 2H), 8.06 (d, J=2.7 Hz, 1H), 8.41 (d, J=2.7 Hz, 1H). |
|
With sulfuric acid; nitric acid; In water; at -30 - 10℃; for 0.5h; |
Example 1A (20g, 87.3 mmol) was cooled to -5 C and treated dropwise with H2SO4(100 mL) at such a rate as to maintain the internal temperature below 10 C. The reactionmixture was cooled to -30 C and treated dropwise with nitric acid (5.7 mL, 91.7 mmol) atsuch a rate as to maintain the internal temperature below -12 C. After the addition wascomplete the reaction flask was placed in an ice bath for 30 minutes and poured onto crushed ice. The resulting suspension was extracted twice with diethyl ether and the combinedextracts were washed with aqueous NaHCOs and brine, dried (MgSO4), filtered, andconcentrated to give 23g of a mixture of methyl 3-bromo-2-methyl-5-nitrobenzoate andmethyl 3-bromo-2-methyl-6-nitrobenzoate. Substitution of this mixture for Example 1C inExample ID followed by purification by silica gel chromatography with 10 to 40% ethylacetate/hexanes provided the desired product. |
- 2
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[ 76006-33-2 ]
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[ 885519-05-1 ]
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[ 894351-65-6 ]
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