HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanesulfonic Acid → HCID 21253070, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanesulfonic Acid | HCID 6395 | — |
| Reactant | HCID 21253071 | HCID 21253071 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 21253070 | HCID 21253070 | 17.2% |
Reaction Steps
A solution of the product from Example 27 (185 mg, 0.44 mmol) in DMF (3 mL) was treated with methane sulfonic acid (30 μL, 0.46 mmol) and stirred at room temperature for 40 hours. The solids were filtered off, washed with DMF and dried to give the first batch of the title compound (39 mg) as a grey solid. The filtrate was concentrated under vacuum, triturated with acetone. The precipitate was then filtered and dried to give the second batch of the title compound (104 mg) as a pale yellow solid, mp=220-225° C., 46% total yield.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06057313 |
| Source dataset | uspto-grants-2000_05 |
| ORD ID | ord-144fc6fc57484a07a8ed732c8c9003dd |
| Source note | uspto-grants-2000_05 |