Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | HCID 66611181 | HCID 66611181 | — |
| Product | HCID 66611809 | HCID 66611809 | — |
Reaction Steps
To a solution of (5-(4-(bis(4-methoxybenzyl)amino)-6-methyl-1,3,5-triazin-2-yl)-6-(5-fluoro-6-methoxypyridin-3-ylamino)pyridin-3-yl)-2,2,2-trifluoroethanol (1.03 g, 1.547 mmol) in dichloromethane (20 mL, 1.547 mmol) was added triethylamine (0.539 mL, 3.87 mmol) and methanesulfonyl chloride (0.244 mL, 3.09 mmol) at 0° C. and the mixture was stirred at the same temperature for 3 h, and warmed up to room temperature and stirred for another 2 h. The reaction was quenched with saturated aqueous NH4Cl solution and water at room temperature, and the separated aqueous layer was extracted with DCM (2×50 mL) and the combined organic layers were dried over Na2SO4 and concentrated and dried under vacuum to give the crude product. m/z (ESI, +ve ion) 684 (M+H)+. The material was used directly without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08362241B2 |
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| Source dataset | uspto-grants-2013_01 |
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| ORD ID | ord-510fae27bf7143cab961912f8a3ec86e |
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| Source note | uspto-grants-2013_01 |
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