HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methylamine hydrochloride → HCID 86687950, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methylamine hydrochloride | HCID 6364545 | — |
| 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 | 8-Amino-2,3-dihydrobenzo[b][1,4]dioxine-5-carboxylic acid | HCID 21193470 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 86687950 | HCID 86687950 | 117.1% |
Reaction Steps
A 50-mL round bottom flash was charged with 8-amino-2,3-dihydrobenzo[b][1,4]dioxine-5-carboxylic acid (200 mg, 1.025 mmol), methylamine hydrochloride (138 mg, 2.05 mmol), HATU (467 mg, 1.23 mmol), TEA (0.5 mL), and DMF (5.0 mL). The reaction mixture was stirred at room temperature for 15 h. It was then purified by reverse-phase Combi-Flash eluting with 0.1% NH4HCO3 in water/CH3CN to afford the title compound as red oil (250 mg, 88%). LCMS: ESI (3 minute run), m/z=209.1 [M+1]+; Retention time: 1.53 minute.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08809331B2 |
| Source dataset | uspto-grants-2014_08 |
| ORD ID | ord-9f4d3ce436814c5aa8b25e13019a9d95 |
| Source note | uspto-grants-2014_08 |