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

Hydrochloric Acid → (S)-tert-butyl 1-oxo-1-(quinolin-3-yl)propan-2-ylcarbamate

HRID 13152
Notes
Print preview

Reaction equation

HRID 13152 reaction equation
CON(C)[C:4](=[O:15])[C@@H:5]([NH:7][C:8](=[O:14])[O:9][C:10]([CH3:13])([CH3:12])[CH3:11])[CH3:6].C([Mg]Cl)(C)C.Br[C:23]1[CH:24]=[N:25][C:26]2[C:31]([CH:32]=1)=[CH:30][CH:29]=[CH:28][CH:27]=2.Cl>C1COCC1.C1COCC1.CCCCCC.CCOC(C)=O>[O:15]=[C:4]([C:23]1[CH:24]=[N:25][C:26]2[C:31]([CH:32]=1)=[CH:30][CH:29]=[CH:28][CH:27]=2)[C@@H:5]([NH:7][C:8](=[O:14])[O:9][C:10]([CH3:11])([CH3:12])[CH3:13])[CH3:6]
ParticipantsConditionsProcedureWorkupSources & evidenceReaction notes

Participants

8

Reactant 4

HCID 313Hydrochloric AcidHCID 214133-BromoquinolineHCID 11806530(S)-tert-Butyl (1-(methoxy(methyl)amino)-1-oxopropan-2-yl)carbamateHCID 178418918HCID 178418918, compound

Product 1

HCID 59339907(S)-tert-butyl 1-oxo-1-(quinolin-3-yl)propan-2-ylcarbamate

Reagents, catalysts & solvents 3

HCID 8028
Tetrahydrofuran
Solvent
2×
HCID 8857Ethyl AcetateSolvent
HCID 21883165Tetrahydrofuran hexaneSolvent

Conditions

Temperature
-10 °C

Procedure

(S)-tert-butyl 1-(methoxy(methyl)amino)-1-oxopropan-2-ylcarbamate (2.5 g, 10.76 mmol) was suspended in THF (5 mL) and stirred at −10° C., isopropylmagnesium chloride 2.0M solution in THF (5.4 ml, 10.80 mmol) was added and a solution was formed. To this solution was added a solution of Lithium tri(3-quinolinyl)magnesiate in THF/Hexane, prepared from 3-bromoquinoline (1.471 ml, 10.81 mmol) according to the procedure described by Sylvain Dumouchel et-al. in Tetrahedron 59 (2003) 8629-8640. The mixture was stirred at −10° C. for 30 min and was the allowed to reach r.t. and stirred over night, 15 h. The reaction mixture, a clear red solution, was slowly poured into ice-cooled 1M HCl (aq) (100 mL). EtOAc (150 mL) was added and the mixture was stirred for a few min, the water phase was extracted once with EtOAc, the combined EtOAc solutions was further washed with saturated NaHCO3 (aq) and brine. The crude material was purified by flash-chromatography on silica using a gradient of 0% to 40% EtOAc in Heptane. The obtained material was the further purified by HPLC to afford the subtitle compound as a yellow sticky oil. Yield 1.6 g (49%)

Workup

  1. customa solution was formed
  2. stirringThe mixture was stirred at −10° C. for 30 min
  3. customto reach r.t.
  4. stirringstirred over night, 15 h
  5. additionThe reaction mixture, a clear red solution, was slowly poured into ice-
  6. stirringthe mixture was stirred for a few min
  7. extractionthe water phase was extracted once with EtOAc
  8. washthe combined EtOAc solutions was further washed with saturated NaHCO3 (aq) and brine
  9. customThe crude material was purified by flash-chromatography on silica using a gradient of 0% to 40% EtOAc in Heptane
  10. customfurther purified by HPLC

Sources & evidence

ORD record
ord-e8677d9cda1d48b590ebce478e9d99c8
Source dataset
uspto-grants-2010_06
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US07728030B2

Reaction notes

Loading…

On this pageParticipantsConditionsProcedureWorkupSources & evidenceReaction notes