HomeMCPWorkbenchSkills
HomeWorkbenchNotificationsMe
llms.txt · MCP GuidePrivacy Policy · Terms of Service · Supportv1.8.0
  1. Home
  2. /Reaction

Dimethylformamide → N6-Methoxy-7-benzyloxy-4-chloro-6-quinolinecarboxamide

HRID 1433740
Notes
Print preview

Reaction equation

HRID 1433740 reaction equation
S(Cl)(Cl)=O.CN(C)C=O.[CH2:10]([O:17][C:18]1[CH:27]=[C:26]2[C:21]([C:22](=O)[CH:23]=[CH:24][NH:25]2)=[CH:20][C:19]=1[C:29]([O:31]C1C=CC=CC=1)=O)[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1.[ClH:38].[O:39]([NH2:41])[CH3:40]>C(OCC)(=O)C.CCCCCC.O>[CH3:40][O:39][NH:41][C:29]([C:19]1[CH:20]=[C:21]2[C:26](=[CH:27][C:18]=1[O:17][CH2:10][C:11]1[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=1)[N:25]=[CH:24][CH:23]=[C:22]2[Cl:38])=[O:31]
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

8

Reactant 4

HCID 6228DimethylformamideHCID 24386Thionyl ChlorideHCID 521874O-Methylhydroxylamine hydrochlorideHCID 22936353Phenyl 7-benzyloxy-4-oxo-1,4-dihydro-6-quinolinecarboxylate

Product 1

HCID 22936829N6-Methoxy-7-benzyloxy-4-chloro-6-quinolinecarboxamideYield 18.2%

Reagents, catalysts & solvents 3

HCID 962WaterSolvent
HCID 8058HexaneSolvent
HCID 8857Ethyl AcetateSolvent2×

Procedure

After adding thionyl chloride (10 ml) and a catalytic amount of dimethylformamide to phenyl 7-benzyloxy-4-oxo-1,4-dihydro-6-quinolinecarboxylate (2.32 g, 6.25 mmol), the mixture was heated to reflux for 2 hours while stirring. The reaction solution was concentrated under reduced pressure and azeotropically distilled twice with toluene, the residue was dissolved in a dimethylformamide (20 ml) and triethylamine (20 ml) mixed solvent, methoxylamine hydrochloride (10.4 g, 125 mmol) was added thereto while cooling in an ice water bath, and the mixture was stirred at room temperature for 18 hours. The reaction solution was distributed between ethyl acetate and water, and then the organic layer was washed with water and saturated brine and dried over anhydrous magnesium sulfate. After distilling off the solvent, it was subjected to silica gel column chromatography, the target fraction was concentrated under reduced pressure, the obtained crude product was suspended in ethyl acetate, the suspension was diluted with hexane, and the crystals were filtered out, washed with hexane and blow-dried to obtain the title compound (392 mg, 1.14 mmol, 18%) as white crystals.

Workup

  1. temperatureto reflux for 2 hours
  2. concentrationThe reaction solution was concentrated under reduced pressure
  3. distillationazeotropically distilled twice with toluene
  4. dissolutionthe residue was dissolved in a dimethylformamide (20 ml) and triethylamine (20 ml)
  5. additionwas added
  6. temperaturewhile cooling in an ice water bath
  7. stirringthe mixture was stirred at room temperature for 18 hours
  8. washthe organic layer was washed with water and saturated brine
  9. dry with materialdried over anhydrous magnesium sulfate
  10. distillationAfter distilling off the solvent, it
  11. concentrationthe target fraction was concentrated under reduced pressure
  12. customthe obtained crude product
  13. filtrationthe crystals were filtered out
  14. washwashed with hexane
  15. customblow-dried

Sources & evidence

ORD record
ord-cc578f4df7324b35887297a9a213aa63
Source dataset
uspto-grants-2009_11
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US07612092B2

Reaction notes

Loading…

On this pageParticipantsProcedureWorkupSources & evidenceReaction notes