HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methylamine → HCID 10346473, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methylamine | HCID 6329 | — |
| Reactant | HCID 22291830 | HCID 22291830 | — |
| Solvent | Dimethylacetamide | HCID 31374 | — |
| Product | HCID 10346473 | HCID 10346473 | — |
Reaction Steps
The title compound was synthesized from N-methylamine (6 mL of 33 w % solution in EtOH) and the compound of Example 216 (1.04 g) by the same procedure used for Example 207 except that 1 mL of DMA was added. The reaction was carried out at 82° C. for 5 days. The title compound, isolated by preparative HPLC, is a white solid (0.29 g, 52%), M.p. 269-270° C. (decomposition). Its structure was confirmed by 1H NMR and LC/MS: 1H NMR (d6-DMSO): δ 2.76 (d, 3H, J=5.5 Hz), 2.84-3.99 (m, 4H), 6.16 (s, 2H), 6.57 (d, 1H, J=9 Hz), 6.91-7.04 (m, 3H), 7.12 (d, 1H, J=1 Hz), 7.22-7.34 (m, 3H), 7.46-7.54 (m, 3H), 10.19 (s, 1H). ESI mass spectrum for C26H22ClN6O4+: 517 (M+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06956052B2 |
| Source dataset | uspto-grants-2005_10 |
| ORD ID | ord-0fae031ac99042fb995ce37b42ceae4e |
| Source note | uspto-grants-2005_10 |