HuagongsheHuagongshe Chemistry Print Report · For research reference only
Isopropylamine → HCID 43693948, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Isopropylamine | HCID 6363 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | HCID 3681313 | HCID 3681313 | — |
| Reactant | Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1) | HCID 9886157 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 43693948 | HCID 43693948 | 60.1% |
Reaction Steps
A solution of 3-benzylamino-benzoic acid (500 mg, 1.5 mmol), HATU (832 mg, 2 mmol), diisopropylethylamine (0.38 ml, 2 mmol) and isopropylamine (0.19 ml, 2 mmol) in acetonitrile was heated to 50° C. for 16 hrs. On cooling, solvents were removed in vacuo and the residue partitioned between dichloromethane and water (50 ml/50 ml). The organic layer was separated, dried over magnesium sulfate and concentrated in vacuo. The residue was purified by column chromatography (ethyl acetate/dichloromethane 0% to 50% v/v) to afford the title compound as a white solid (242 mg). HPLC retention time 2.69 min. Mass spectrum (ES+) m/z 269.9 (M+H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09447033B2 |
| Source dataset | uspto-grants-2016_09 |
| ORD ID | ord-3635c692fd4448fc83af8193396e8ad9 |
| Source note | uspto-grants-2016_09 |