HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 71087465, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | hydroxylamine-O-sulfonic acid | HCID 76284 | — |
| Reactant | HCID 86674739 | HCID 86674739 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 71087465 | HCID 71087465 | 97.1% |
Reaction Steps
A mixture of tert-butyl 1-(1-(dimethylamino)ethylideneamino)-2-methyl-1-thioxopropan-2-ylcarbamate (2.9 g, 10 mmol), hydroxylamine-O-sulfonic acid (CAN 2950-43-8, 1.37 g, 12 mmol), pyridine (1.6 g, 20.2 mmol) and methanol (4 mL) in ethanol (20 mL) was stirred at room temperature for 2 h. After evaporation of solvents, the residue was diluted with ethyl acetate (40 mL) and water (40 mL). The organic layer was washed with brine (40 mL), dried over anhydrous sodium sulfate and concentrated to give crude product (2.5 g, 96%) as yellow oil. The product was used directly in the next step without further purification; MS (EI): m/e 258.2 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09321727B2 |
| Source dataset | uspto-grants-2016_04 |
| ORD ID | ord-efe16bb89fc54475b89ed7b64def5e85 |
| Source note | uspto-grants-2016_04 |