Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 3-(4,6-Dimethoxy-1,3,5-triazin-2-yl)-7-fluoroindolin-2-one | HCID 67982437 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 67983090 | HCID 67983090 | — |
Reaction Steps
3-(4,6-Dimethoxy-1,3,5-triazin-2-yl)-7-fluoro-1,3-dihydro-2H-indol-2-one (5.0 g) is introduced as initial charge in 225 ml of acetonitrile, sodium hydride (0.73 g, 60% in mineral oil) is added and the mixture is after-stirred until a thick suspension is formed. After adding iodomethane (7.0 g), the mixture is heated to 60° C. and stirred for 11 hours at 60° C. The organic solvent is largely distilled off in vacuo. 2-Propanol is added to the partially crystalline residue and the product is filtered off. This gives the intermediate as a solid in an HPLC purity of 93% (3.46 g, 64% of theory). The structure can be confirmed by NMR spectroscopy.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08969553B2 |
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| Source dataset | uspto-grants-2015_03 |
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| ORD ID | ord-1f468e9bd36944c5849fde1d36bc9256 |
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| Source note | uspto-grants-2015_03 |
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