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Oxalyl chloride → 2,3-Dichloroaniline

HRID 253950
Notes
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Reaction equation

HRID 253950 reaction equation
[F:1][C:2]1[N:10]=[CH:9][CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].C(Cl)(=O)C(Cl)=O.FC1C(F)=CC=CC=1N.C([O-])(O)=O.[Na+].C(NC1C(C([NH:44][C:45]2[CH:50]=[CH:49][CH:48]=[C:47]([Cl:51])[C:46]=2[Cl:52])=O)=CC=CN=1)(C)(C)C.C(NC1C(C([NH:66][C:67]2[CH:72]=[CH:71][CH:70]=[C:69]([Cl:73])[C:68]=2[F:74])=O)=CC=CN=1)(C)(C)C>C(Cl)Cl.C(N(CC)CC)C.CN(C=O)C>[F:1][C:2]1[N:10]=[CH:9][CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].[Cl:52][C:46]1[C:47]([Cl:51])=[CH:48][CH:49]=[CH:50][C:45]=1[NH2:44].[Cl:73][C:69]1[C:68]([F:74])=[C:67]([CH:72]=[CH:71][CH:70]=1)[NH2:66]
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

12

Reactant 6

HCID 65578Oxalyl chlorideHCID 782782,3-DifluoroanilineHCID 960892-Fluoronicotinic acidHCID 516892Sodium BicarbonateHCID 668663562-(tert-butylamino)-N-(2,3-dichlorophenyl)pyridine-3-carboxamideHCID 668679862-(tert-butylamino)-N-(3-chloro-2-fluorophenyl)pyridine-3-carboxamide

Product

3
HCID 118442,3-DichloroanilineHCID 750143-Chloro-2-fluoroanilineHCID 960892-Fluoronicotinic acid

Reagents, catalysts & solvents 3

HCID 6228DimethylformamideSolventHCID 6344DichloromethaneSolventHCID 8471TriethylamineSolvent

Procedure

A room temperature solution of 2-fluoronicotinic acid (1 g) in DCM (20 mL) was sequentially treated with DMF (0.2 mL) and oxalyl chloride (0.62 mL, 1 eq). The resulting solution was stirred at RT for 1 hour and monitored by HPLC (analyte quenced with methanol) until the consumption of starting material was complete. The reaction mixture was cooled to 0° C. and sequentially treated with 2,3-difluoroaniline (1.4 g, 1.5 eq) and 2 mL of triethylamine. The reaction was warmed to RT and maintained for 3 additional hours, followed by washing the mixture with 2N HCl, saturated NaCl, and saturated NaHCO3 solution. The organic extracts were dried over MgSO4, filtered, and concentrated in vacuo. The resulting crude 2-fluoro-N-(2,3-difluorophenyl)pyridine-3-carboxamide was dissolved in NMP (20 mL) and reacted with excess t-butylamine at 80° C. for 14 hours. After cooling to RT, the solution was poured into sat NaHCO3 solution. The resulting precipitate was collected by filtration and washed with water. The crude product, 2-(tert-butylamino)-N-(2,3-difluorophenyl)pyridine-3-carboxamide, was dried in vacuo and used directly in the next reaction without further purification. Using the same procedure, 2-(tert-butylamino)-N-(2,3-dichlorophenyl)pyridine-3-carboxamide and 2-(tert-butylamino)-N-(3-chloro-2-fluorophenyl)pyridine-3-carboxamide can be produced from the reaction of 2-fluoronicotinic acid with 2,3-dichloroaniline and 3-chloro-2-fluoroaniline, respectively.

Workup

  1. custommonitored by HPLC (analyte quenced with methanol) until the consumption of starting material
  2. temperatureThe reaction mixture was cooled to 0° C.
  3. temperatureThe reaction was warmed to RT
  4. temperaturemaintained for 3 additional hours
  5. washby washing the mixture with 2N HCl, saturated NaCl, and saturated NaHCO3 solution
  6. dry with materialThe organic extracts were dried over MgSO4
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo
  9. dissolutionThe resulting crude 2-fluoro-N-(2,3-difluorophenyl)pyridine-3-carboxamide was dissolved in NMP (20 mL)
  10. customreacted with excess t-butylamine at 80° C. for 14 hours
  11. temperatureAfter cooling to RT
  12. additionthe solution was poured
  13. filtrationThe resulting precipitate was collected by filtration
  14. washwashed with water
  15. dry with materialThe crude product, 2-(tert-butylamino)-N-(2,3-difluorophenyl)pyridine-3-carboxamide, was dried in vacuo
  16. customused directly in the next reaction without further purification

Sources & evidence

ORD record
ord-2945f749b62946f08d1ec5096eaa4ea7
Source dataset
uspto-grants-2011_01
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US07872031B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes