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

Methyl iodide → 5-Acetyl-4-cyclohexyl-2-methylsulfanyl-thiophene-3-carbonitrile

HRID 6859
Notes
Print preview

Reaction equation

HRID 6859 reaction equation
[CH:1]1([C:7](=O)[CH2:8][C:9]#[N:10])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.C([O-])([O-])=O.[K+].[K+].Cl[CH2:19][C:20](=[O:22])[CH3:21].I[CH3:24].CN(C=O)C.[C:30](=[S:32])=[S:31]>>[C:20]([C:19]1[S:31][C:30]([S:32][CH3:24])=[C:8]([C:9]#[N:10])[C:7]=1[CH:1]1[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1)(=[O:22])[CH3:21]
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

6

Reactant 5

HCID 6328Methyl iodideHCID 6571ChloroacetoneHCID 11430Potassium CarbonateHCID 113095973-Cyclohexyl-3-oxopropanenitrileHCID 86590990Dmf CS2

Product 1

HCID 220190435-Acetyl-4-cyclohexyl-2-methylsulfanyl-thiophene-3-carbonitrile

Procedure

To a solution of 3-cyclohexyl-3-oxo-propionitrile in DMF:CS2 (1:1) was added K2CO3 at 0° C. and the reaction mixture stirred at ambient temperature for 2 hours. To the resulting reaction mixture was added chloroacetone (1 equivalent) and the reaction mixture stirred at ambient temperature for 3 hours. Iodomethane was then added and the resulting mixture was stirred at ambient temperature overnight. The reaction mixture was partitioned between ethyl acetate and brine, the organic phase dried with MgSO4 and the solvent was removed under reduced pressure. The crude product was purified by silica gel chromatography.

Workup

  1. customTo the resulting reaction mixture
  2. stirringthe reaction mixture stirred at ambient temperature for 3 hours
  3. stirringthe resulting mixture was stirred at ambient temperature overnight
  4. customThe reaction mixture was partitioned between ethyl acetate and brine
  5. dry with materialthe organic phase dried with MgSO4
  6. customthe solvent was removed under reduced pressure
  7. customThe crude product was purified by silica gel chromatography

Sources & evidence

ORD record
ord-183102cc420b4877ac00ee09af6bc6a9
Source dataset
uspto-grants-2006_08
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US07084159B2

Reaction notes

Loading…

On this pageParticipantsProcedureWorkupSources & evidenceReaction notes