HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Anhydride → HCID 131730972, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Anhydride | HCID 7918 | — |
| Reactant | Azane;hydrate | HCID 12896473 | — |
| Reactant | HCID 131730953 | HCID 131730953 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 131730972 | HCID 131730972 | 73% |
Reaction Steps
25 mg of 4-(benzylamino)-6-{[4-(1,4-diazepan-1-yl)phenyl]amino}pyridine-3-carboxyamide (the compound of Example 226) was dissolved in 1.5 mL of dichloromethane, to which, under ice cooling, 15.1 mg of acetic anhydride was added, and stirred for 30 minutes. To the reaction mixture 1.5 mL of ammonia water was added, extracted with chloroform, 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=10:1), recrystallized from chloroform-methanol-diethylether to obtain 20 mg (73%) of the title compound as light brown needle crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08575153B2 |
| Source dataset | uspto-grants-2013_11 |
| ORD ID | ord-df692708b6e54fcfabd95b326f641f3e |
| Source note | uspto-grants-2013_11 |