HuagongsheHuagongshe Chemistry Print Report · For research reference only
Aniline → HCID 59207989, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Aniline | HCID 6115 | — |
| Reactant | Methanaminium, N-((1H-benzotriazol-1-yloxy)(dimethylamino)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1) | HCID 2733084 | — |
| Reactant | HCID 59208014 | HCID 59208014 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 59207989 | HCID 59207989 | 35% |
Reaction Steps
To the solution of 3-(8-(2,6-difluorophenyl)-2-{[2-(dimethylamino)ethyl]-amino}-7-oxo-5,6,7,8-tetrahydropyrimido[4,5-d]pyrimidin-4-yl)-5-fluoro-4-methylbenzoic acid (25 mg, 0.05 mmol) in CH2Cl2 (2 mL) were added aniline (0.025 mL, 0.25 mmol) and HBTU (20 mg, 0.053 mmol). The reaction mixture was stirred over night. The reaction mixture was concentrated. Separation via a HPLC with TFA followed by treatment with t-amino SPE cartridge then provided the title compound as a white solid (10 mg, 35%). LC-MS m/z 576 (M+H)+; 1H-NMR (MeOD) δ 2.27 (s, 3H), 2.79 (s, 6H), 3.15 (m, 2H), 3.55 (m, 2H), 4.21 (s, 2H), 7.19 (m, 3H), 7.39 (m, 2H), 7.54 (m, 1H), 7.71 (m, 3H), 7.86 (m, 1H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07674789B2 |
| Source dataset | uspto-grants-2010_03 |
| ORD ID | ord-3d2ed009162a4348bf3c3af031fa12e7 |
| Source note | uspto-grants-2010_03 |