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[ CAS No. 29124-62-7 ]

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Chemical Structure| 29124-62-7
Chemical Structure| 29124-62-7
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Product Details of [ 29124-62-7 ]

CAS No. :29124-62-7 MDL No. :MFCD00672936
Formula : C9H7BrF3NO Boiling Point : -
Linear Structure Formula :- InChI Key :N/A
M.W :282.06 g/mol Pubchem ID :-
Synonyms :

Safety of [ 29124-62-7 ]

Signal Word:Warning Class:N/A
Precautionary Statements:P261-P264-P271-P280-P302+P352-P304+P340+P312-P305+P351+P338-P332+P313-P337+P313-P362-P403+P233-P405-P501 UN#:N/A
Hazard Statements:H315-H319-H335 Packing Group:N/A
GHS Pictogram:

Application In Synthesis of [ 29124-62-7 ]

  • Upstream synthesis route of [ 29124-62-7 ]
  • Downstream synthetic route of [ 29124-62-7 ]

[ 29124-62-7 ] Synthesis Path-Upstream   1~1

  • 1
  • [ 29124-62-7 ]
  • [ 157026-18-1 ]
YieldReaction ConditionsOperation in experiment
99%
Stage #1: at 5 - 12℃;
Stage #2: With hydrogenchloride In methanol; water at 100℃;
Step B4-bromo-2-nitro-6-(trifluoromethyl)aniline[00234] Sulfuric acid (350 ml) was cooled to 5 °C in an ice-bath before V-[4-bromo-2- (trifluoromethyl)phenyl]acetamide (100 g, 355 mmol) was added portion-wise. The observed internal temperature increased from 5 °C to 10 °C. After the solids dissolved and temperature decreased to 5 °C, nitric acid (70percent) (43.8 ml) was added slowly drop-wise at such a rate that the internal temperature did not increase above 10 °C. The temperature was carefully controlled between 8 °C and 12 °C until the reaction was complete. The cold dark solution was carefully poured into stirring ice water (2L, mostly ice). The tan precipitate was collected by filtration and the filter cake washed with 1 L of cold water before being air dried. The tan powder was slurried in methanol (500 mL) in a 3L 3-neck flask, and concentrated hydrochloric acid (37percent) (750 mL, 9130 mmol) was added and the mixture heated with a heating mantel to 100 °C. Excessive frothing occurred. 10OmL of 1 ,4-dioxane and 200mL of tetrahydrofuran were added to help the frothing subside. Frothing did not subside. The reaction temperature was brought down to 80 °C and heated overnight. The mixture was much more manageable and frothing was better controlled. The mixture was slowly heated to 95 °C and was stirred for 72 hours. The mixture was cooled to room temperature and extracted 3 times with ethyl acetate. The combined organic layers were washed with brine, dried over sodium sulfate, and concentrated to give the title compound (101 g, 99percent). 1H NMR (400 MHz, DMSO-tf6) δ ppm 8.40 (d, 1 H), 7.96 (d, 1 H), 7.44 (br. s 2 H).
Reference: [1] Patent: WO2011/97491, 2011, A1, . Location in patent: Page/Page column 117-118
[2] Journal of Medicinal Chemistry, 1995, vol. 38, # 22, p. 4367 - 4379
[3] Patent: WO2011/97491, 2011, A1,
[4] Patent: US5514680, 1996, A,
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