HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diisopropylethylamine → HCID 66648757, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 3-Chloro-6-methylpyridazine | HCID 227254 | — |
| Reactant | HCID 24956161 | HCID 24956161 | — |
| Product | HCID 66648757 | HCID 66648757 | 26.6% |
Reaction Steps
A mixture of Example 12 (44 mg, 0.134 mmol), 3-chloro-6-methylpyridazine (15 mg, 0.116 mmol) and DIPEA (0.5 mL, 67.0 mmol) was heated to 180° C. under microwave irradiation for 2 h. A further portion of 3-chloro-6-methylpyridazine (15 mg, 0.116 mmol) was added and heating continued for a further 20 h. The solvent was removed in vacuo and the residue purified by prep HPLC to give the title compound (13 mg, 23%) as a yellow solid. δH (CDCl3) 1.15 (6H, s), 2.42 (2H, s), 2.58 (3H, s), 2.76 (2H, s), 4.13-4.18 (2H, m), 4.32-4.38 (2H, m), 6.93-7.20 (5H, m), 8.03 (1H, d, J 2.4 Hz). LCMS (ES+) 422 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08093238B2 |
| Source dataset | uspto-grants-2012_01 |
| ORD ID | ord-21fcfb2fd61a417896a480eea61976b0 |
| Source note | uspto-grants-2012_01 |