HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 131730956, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | 2-Bromoethyl methyl ether | HCID 80972 | — |
| Reactant | HCID 131730957 | HCID 131730957 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 131730956 | HCID 131730956 | 30.5% |
Reaction Steps
37 mg of 6-[(4-aminophenyl)amino]-4-[(3,5-difluorobenzyl)amino]pyridine-3-carboxyamide (the compound of Example 67) and 14 mg of 2-bromoethyl methylether were dissolved in 0.3 mL of N,N-dimethylformamide, and stirred using a microwave reaction apparatus under an argon atmosphere at 120° C. for 20 minutes. After cooling, water was added to the reaction mixture, extracted with ethyl acetate, the extract was washed with saturated saline, and dried on anhydrous sodium sulfate. The solvent was evaporated, and the residue was purified by silica gel thin layer chromatography (chloroform:methanol=20:1, developed twice) to obtain 13 mg (yield: 29%) of the title compound as a light yellow solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08575153B2 |
| Source dataset | uspto-grants-2013_11 |
| ORD ID | ord-c30d14b1bab34e3aa9798fc01d614f52 |
| Source note | uspto-grants-2013_11 |