HuagongsheHuagongshe Chemistry Print Report · For research reference only
1-Methylpiperazine → Ammonium Hydroxide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1-Methylpiperazine | HCID 53167 | — |
| Reactant | HCID 11950625 | HCID 11950625 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | Ammonium Hydroxide | HCID 14923 | — |
| Product | HCID 59208129 | HCID 59208129 | — |
Reaction Steps
3-[8-(2,6-difluorophenyl)-2-(methylsulfonyl)-7-oxo-5,6,7,8-tetrahydropyrimido[4,5-d]pyrimidin-4-yl]-N,N,4-trimethylbenzamide (0.050 g, 0.1 mmol) was dissolved in THF (5 mL) and 1-methylpiperazine (0.050 g, 0.5 mmol) was added. The reaction was stirred under argon overnight. The solvents were pumped off in vacuo. The residue was flash chromatographed on silica gel (15 g) eluted with CH2Cl2 to 6:0.5:0.05, CH2Cl2:ethanol:NH4OH to give the title compound as a white amorphous solid. mp 159-162° C. LC-MS m/z 522 (M+H)+, 1.59 min (ret time).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07674789B2 |
| Source dataset | uspto-grants-2010_03 |
| ORD ID | ord-0af9afc8a8764f4da721a845ecbd198e |
| Source note | uspto-grants-2010_03 |