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

HCID 67097724, compound → Methyl 4-amino-2-oxo-1,2-dihydroquinoline-3-carboxylate

HRID 2077013
Notes
Print preview

Reaction equation

HRID 2077013 reaction equation
COC1C=CC(C[NH:8][C:9]2[C:18]3[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=3)[NH:12][C:11](=[O:19])[C:10]=2[C:20]([O:22][CH3:23])=[O:21])=CC=1>C(O)(C(F)(F)F)=O>[NH2:8][C:9]1[C:18]2[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=2)[NH:12][C:11](=[O:19])[C:10]=1[C:20]([O:22][CH3:23])=[O:21]
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

3

Reactant 1

HCID 67097724HCID 67097724, compound

Product 1

HCID 658173Methyl 4-amino-2-oxo-1,2-dihydroquinoline-3-carboxylateYield 42.3%

Reagents, catalysts & solvents 1

HCID 6422Trifluoroacetic acidSolvent

Procedure

Methyl 4-(4-methoxybenzylamino)-2-oxo-1,2-dihydroquinoline-3-carboxylate (Example 68a) (0.841 g, 2.49 mmol) was dissolved in TFA (5 mL) and stirred at room temperature for 30 minutes. The TFA was removed under reduced pressure, and the residue was dissolved in dichloromethane, then precipitated out by adding excess diethyl ether. The resultant solid was collected by filtration, suspended in dichloromethane, and washed with concentrated sodium bicarbonate. The solid was collected to give methyl 4-amino-2-oxo-1,2-dihydroquinoline-3-carboxylate (0.230 g, 42%) as a white solid. M.p.: 236° C. 1H NMR (400 MHz, DMSO-d6) δ 3.73 (s, 3H), 7.12 (t, J=8.0 Hz, 1H), 7.17 (d, J=8.0 Hz, 1H), 7.52 (t, J=8.0 Hz, 1H), 8.08 (d, J=8.0 Hz, 1H), 8.38 (bs, 2H), 10.88 (bs, 1H). MS 219 (MH+).

Workup

  1. customThe TFA was removed under reduced pressure
  2. dissolutionthe residue was dissolved in dichloromethane
  3. customprecipitated out
  4. additionby adding excess diethyl ether
  5. filtrationThe resultant solid was collected by filtration
  6. washwashed with concentrated sodium bicarbonate
  7. customThe solid was collected

Sources & evidence

ORD record
ord-41b2e65c30e84be9b6870cd557bb414d
Source dataset
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US07928111B2

Reaction notes

Loading…

On this pageParticipantsProcedureWorkupSources & evidenceReaction notes