HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetyl chloride → HCID 86696397, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetyl chloride | HCID 6367 | — |
| Reactant | HCID 86696395 | HCID 86696395 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 86696397 | HCID 86696397 | 20% |
Reaction Steps
To a solution of tert-butyl 4-(6-(butylamino)imidazo[1,2-b]pyridazine-3-carboxamido)benzylcarbamate (230 mg, 0.53 mmol) in methanol (15 mL) was added acetyl chloride (0.37 mL, 5.25 mmol) dropwise. The reaction mixture was stirred for overnight, concentrated and purified by Prep HPLC (neutral) to give N-(4-(aminomethyl)phenyl)-6-(butylamino)imidazo[1,2-b]pyridazine-3-carboxamide (25 mg, 20% yield). 1H NMR (400 MHz, METHANOL-d4) δ ppm 8.54 (s, 1H), 8.11 (s, 1H), 7.80 (d, J=8.38 Hz, 2H), 7.77 (d, J=9.92 Hz, 1H), 7.50 (d, J=8.38 Hz, 2H), 6.92 (d, J=9.70 Hz, 1H), 4.12 (s, 2H), 3.48 (t, J=7.17 Hz, 2H), 1.79 (quin, J=7.33 Hz, 2H), 1.55 (dq, J=15.02, 7.41 Hz, 2H), 1.02 (t, J=7.39 Hz, 3H); LRMS (ESI) m/e 339.2 [(M+H)+, calcd for C18H23N6O 339.4].
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08969565B2 |
| Source dataset | uspto-grants-2015_03 |
| ORD ID | ord-ce17a29fe145489286b270e7e84714ea |
| Source note | uspto-grants-2015_03 |