HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diisopropylethylamine → HCID 11950624, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1) | HCID 9886157 | — |
| Reactant | 3-[8-(2,6-Difluorophenyl)-2-(methylthio)-7-oxo-5,6,7,8-tetrahydropyrimido[4,5-d]pyrimidin-4-yl]-4-methylbenzoic acid | HCID 11950622 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 11950624 | HCID 11950624 | — |
Reaction Steps
3-[8-(2,6-difluorophenyl)-2-(methylthio)-7-oxo-5,6,7,8-tetrahydropyrimido[4,5-d]pyrimidin-4-yl]-4-methylbenzoic acid (0.59 g, 1.33 mmol) was taken up in CH2Cl2 (75 mL), and diisopropylethylamine (0.7 mL, 4 mmol) was added followed by HATU (0.556 g, 1.46 mmol). Gaseous methyl amine was then bubbled in very slowly until reaction was complete. Aqueous workup followed by chromatography on silica gel (100 g) eluted with CH2Cl2 —90% EtOAc/CH2Cl2 gave the title compound as a white amorphous solid. mp 273-275° C. LC-MS m/z 456 (M+H)+, 1.85 min (ret time).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07674789B2 |
| Source dataset | uspto-grants-2010_03 |
| ORD ID | ord-8c3782dada454e8bbc883b47152905a5 |
| Source note | uspto-grants-2010_03 |