HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanesulfonic Acid → HCID 86608139, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanesulfonic Acid | HCID 6395 | — |
| Reactant | HCID 59730332 | HCID 59730332 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Dichloromethane methanol | HCID 21226129 | — |
| Product | HCID 86608139 | HCID 86608139 | — |
Reaction Steps
Dissolve 6-(4-{[2-(4-fluorophenyl)ethylamino]methyl}-2-methoxyphenoxy)nicotinamide (Example 430) (8.40 g, 2.12 mmol) in dichloromethane:methanol (1:1) (4.25 mL) and add 1 equivalent of 0.50 M methanesulfonic acid in dichloromethane. Stir the solution for a short time before concentrating to give the title compound (0.1.02 g): TOF MS ES+ 396.2 (M+H)+, HRMS calcd for C22H23N3O3.F 396.1723 (M+H)+, found 396.1731, time 0.39 min; HPLC [YMC-Pro pack C-18 (150×4.6 mm, S-5 microm), 0.05% TFA/acetonitrile in 0.05% TFA/water at 1.0 mL/min, 10-20% over 5 min, 20-95% over 18], tR=10.9 min, 100% purity.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07560463B2 |
| Source dataset | uspto-grants-2009_07 |
| ORD ID | ord-ac6e3c59a1024c028350c57d861eed50 |
| Source note | uspto-grants-2009_07 |