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ChemicalBook--->CAS DataBase List--->1150617-94-9

1150617-94-9

1150617-94-9 Structure

1150617-94-9 Structure
IdentificationBack Directory
[Name]

5-Iodo-2-methyl-2H-indazole
[CAS]

1150617-94-9
[Synonyms]

5-iodo-2-methylindazole
5-Iodo-2-methyl-2H-indazole
2H-Indazole, 5-iodo-2-methyl-
[Molecular Formula]

C8H7IN2
[MDL Number]

MFCD11977518
[MOL File]

1150617-94-9.mol
[Molecular Weight]

258.06
Chemical PropertiesBack Directory
[storage temp. ]

Keep in dark place,Sealed in dry,Room Temperature
[Appearance]

Light green to green Solid
Safety DataBack Directory
[Symbol(GHS) ]


GHS07
[Signal word ]

Warning
[Hazard statements ]

H302-H315-H319-H332-H335
[Precautionary statements ]

P280-P305+P351+P338-P310
Spectrum DetailBack Directory
[Spectrum Detail]

5-Iodo-2-methyl-2H-indazole(1150617-94-9)1HNMR
Hazard InformationBack Directory
[Synthesis]

5-Iodo-1H-indazole

55919-82-9

Trimethyloxonium Tetrafluoroborate

420-37-1

5-Iodo-2-methyl-2H-indazole

1150617-94-9

General procedure for the preparation of 5-iodo-2-methyl-2H-indazole: To a solution of 5-iodo-1H-indazole (500 g, 2.05 mol) in ethyl acetate (EtOAc, 4 L) was added trimethoxonium tetrafluoroborate (450 g, 3.04 mol). The resulting white suspension was stirred at room temperature for 2 h and subsequently concentrated under reduced pressure. Water (1 L) was added to the concentrated residue and the pH was adjusted with 10% aqueous sodium hydroxide (NaOH) to 12. The solid was collected by filtration and redissolved in dichloromethane (DCM, 5 L). After filtration to remove insoluble matter, the filtrate was washed with 10% aqueous NaOH (2 × 100 mL). The organic layer was dried with anhydrous sodium sulfate (Na2SO4), filtered through a short silica gel column and concentrated again. Methyl tert-butyl ether was added to the residue to form a slurry and the product was collected by filtration to give the final title compound 5-iodo-2-methyl-2H-indazole (360 g, 68.0% yield). Mass spectrometry (MS) data: m/z 259.0 ([M+H]+).

[References]

[1] Patent: US2012/28984, 2012, A1. Location in patent: Page/Page column 3
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