Methyl iodide → HCID 178504020, compound

HRID 1803141Notes

Reaction equation

HRID 1803141 reaction equation
[I:1][CH3:2].[Cl:3][C:4]1[N:5]=[CH:6][N:7]([C:9]2[C:14]([F:15])=[CH:13][C:12]([NH:16][C:17]([NH2:19])=[S:18])=[CH:11][C:10]=2[F:20])[CH:8]=1>C(O)C>[IH:1].[Cl:3][C:4]1[N:5]=[CH:6][N:7]([C:9]2[C:10]([F:20])=[CH:11][C:12]([NH:16][C:17]([S:18][CH3:2])=[NH:19])=[CH:13][C:14]=2[F:15])[CH:8]=1

Participants

4

Reactant 2

HCID 6328Methyl iodideHCID 86649906HCID 86649906, compound

Product 1

HCID 178504020HCID 178504020, compoundYield 100%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Conditions

Temperature
60 °C

Procedure

Step J (5): Iodomethane (0.047 mL, 0.753 mmol) was added to a solution of 1-(4-(4-chloro-1H-imidazol-1-yl)-3,5-difluorophenyl)thiourea (207 mg, 0.717 mmol) in absolute ethanol (4 mL). The resulting mixture was heated at 60° C. for 16 h. After cooling to rt, the reaction was concentrated in vacuo. The residual volatiles were removed in high vacuo to afford methyl 4-(4-chloro-1H-imidazol-1-yl)-3,5-difluorophenylcarbamimidothioate hydroiodide (309 mg, 0.717 mmol, 100% yield). LC-MS (M+11)+ 303.1.

Workup

  1. temperatureAfter cooling to rt
  2. concentrationthe reaction was concentrated in vacuo
  3. customThe residual volatiles were removed in high vacuo

Sources & evidence

ORD record
ord-d5fc130fc3c94f648ff98bfcc6ad0b1c
Source dataset
uspto-grants-2013_01
Patent number
US08349880B2

Reaction notes

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