HuagongsheHuagongshe Chemistry Print Report · For research reference only
4-Aminopyridine → HCID 44512903, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4-Aminopyridine | HCID 1727 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Triphosgene | HCID 94429 | — |
| Reactant | HCID 67021980 | HCID 67021980 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 44512903 | HCID 44512903 | 29.7% |
Reaction Steps
To a stirred solution of triphosgene (269 mg, 0.90 mmol) in CH2Cl2 (5 mL) was added 3-{[4-(4-Amino-phenyl)-6-morpholin-4-yl-[1,3,5]triazin-2-ylamino]-methyl}-azetidine-1-carboxylic acid tert-butyl ester (500 mg, 1.13 mmol) at 25° C. The reaction mixture was stirred for 15 min and 4-aminopyridine (319 mg, 3.39 mmol) and NEt3 (1.56 mL, 11.3 mmol) were added and the reaction mixture was stirred for additional 1 hr. The solvents were removed on a rotary evaporator and the crude mixture was purified by semi-prep-HPLC (TFA-method) to give 3-({4-Morpholin-4-yl-6-[4-(3-pyridin-4-yl-ureido)-phenyl]-[1,3,5]triazin-2-ylamino}-methyl)-azetidine-1-carboxylic acid tert-butyl ester (150 mg, 16% yield); MS (ESI) m/z 562.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09174963B2 |
| Source dataset | uspto-grants-2015_11 |
| ORD ID | ord-d3102d033bce4a47adefdefeca7cc885 |
| Source note | uspto-grants-2015_11 |