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

N-Iodosuccinimide → 7-Iodo-5-methylimidazo[5,1-b]thiazole

HRID 1839304
Notes
Print preview

Reaction equation

HRID 1839304 reaction equation
[CH3:1][C:2]1[N:9]2[C:5]([S:6][CH:7]=[CH:8]2)=[CH:4][N:3]=1.[I:10]N1C(=O)CCC1=O>ClCCl.IN1C(=O)CCC1=O>[I:10][C:4]1[N:3]=[C:2]([CH3:1])[N:9]2[CH:8]=[CH:7][S:6][C:5]=12
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

5

Reactant 2

HCID 120273N-IodosuccinimideHCID 177738035-Methylimidazo[5,1-b]thiazole

Product 1

HCID 226318267-Iodo-5-methylimidazo[5,1-b]thiazoleYield 105.1%

Reagents, catalysts & solvents 2

HCID 120273N-IodosuccinimideCatalystHCID 6344DichloromethaneSolvent

Procedure

5-Methylimidazo[5,1-b]thiazole (6.90 g) was dissolved in 500 ml of dichloromethane. N-Iodosuccinimide (10.6 g) was added to the solution. The mixture was stirred at room temperature for 24 hr. N-Iodosuccinimide (1.06 g) was added thereto, followed by stirring for additional one hr. The reaction solution was washed with an aqueous sodium thiosulfate solution and brine in that order, dried over anhydrous magnesium sulfate, and then filtered. The solvent was removed by distillation under the reduced pressure. The residue was dissolved in 200 ml of dichloromethane and 100 ml of ethyl acetate. Silica gel (30 g) was added to the solution. The mixture was stirred. The silica gel was removed by filtration. The filtrate was washed with 200 ml of a mixed solution of dichloromethane:ethyl acetate=2:1. The filtrate was concentrated under the reduced pressure to give 13.08 g of 7-iodo-5-methylimidazo[5,1-b]thiazole.

Workup

  1. stirringby stirring for additional one hr
  2. washThe reaction solution was washed with an aqueous sodium thiosulfate solution and brine in that order
  3. dry with materialdried over anhydrous magnesium sulfate
  4. filtrationfiltered
  5. customThe solvent was removed by distillation under the reduced pressure
  6. dissolutionThe residue was dissolved in 200 ml of dichloromethane
  7. additionSilica gel (30 g) was added to the solution
  8. stirringThe mixture was stirred
  9. customThe silica gel was removed by filtration
  10. washThe filtrate was washed with 200 ml of a mixed solution of dichloromethane
  11. concentrationThe filtrate was concentrated under the reduced pressure

Sources & evidence

ORD record
ord-59036cf0891f4f4bb8688adad5b5c976
Source dataset
uspto-grants-2004_01
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US06677331B2

Reaction notes

Loading…

On this pageParticipantsProcedureWorkupSources & evidenceReaction notes