[ CAS No. 1070892-03-3 ]

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Product Details

CAS No. :1070892-03-3MDL No. :MFCD28746889
Formula :C7H4BrF3N2OInChI Key :-
M.W :269.02Pubchem ID :-
Boiling Point :-
Synonyms :

Computed Properties

TPSA : - H-Bond Acceptor Count : -
XLogP3 : - H-Bond Donor Count : -
SP3 : 0.00 Rotatable Bond Count : -

Safety

Signal Word:WarningClassN/A
Precautionary Statements:P261-P305+P351+P338UN#:N/A
Hazard Statements:H302-H315-H319-H335Packing Group:N/A
GHS Pictogram:

Application In Synthesis

[ 1070892-03-3 ] Synthesis Path-Upstream   1~3

  • 1
  • [ 749875-16-9 ]
  • [ 1070892-03-3 ]
YieldReaction ConditionsOperation in experiment
82%
Stage #1: With oxalyl dichloride In dichloromethane at 20℃; for 2.00 h;
Stage #2: With ammonia In water; acetonitrile at 0℃; for 0.33 h;
To a 500 mL round bottom flask equipped with a stir bar, condenser and nitrogen inlet was charged 38.9 g (144 mmol) of δ-bromo^-trifluoromethyl-isonicotinic acid. To the solid was charged 250 mL of anhydrous dichloromethane followed by 13.2 mL (151 mmol, 1.05 eq) oxalyl chloride. To the mixture was added 0.5 mL of anhydrous dimethylformamide and the mixture was stirred at ambient temperature for 2h. The reaction was complete as evidenced by HPLC (methanol quench of aliquot). The solvent was removed in vacuo affording an amber oil.To a 1 L Erlenmeyer flask equipped with a stir bar in an ice-bath was charged 500 mL of aqueous ammonium hydroxide. To the chilled solution was added dropwise the crude acid chloride. The residue was transferred with a small amount of acetonitrile. The mixture was stirred for 20 minutes following addition. The resulting precipitate was collected by filtration and washed with water. The filter cake was dried in vacuo at 45 0C affording 31.8 g of δ-bromo^-trifluoromethyl-isonicotinamide as an off-white solid in a 82percent yield. The compound may also be purified using an ether slurry and collecting the solid.
Reference: [1] Patent: WO2008/124610, 2008, A1. Location in patent: Page/Page column 44; 45
[2] Patent: WO2008/124614, 2008, A1
  • 2
  • [ 1070972-53-0 ]
  • [ 1070892-03-3 ]
Reference: [1] Patent: WO2008/124614, 2008, A1. Location in patent: Page/Page column 36-37
  • 3
  • [ 436799-32-5 ]
  • [ 1070892-03-3 ]
Reference: [1] Patent: WO2008/124614, 2008, A1
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