HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethyl Sulfate → HCID 68765199, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethyl Sulfate | HCID 6497 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | 2-(3-Fluoro-3'-hydroxybiphenyl-4-ylamino)nicotinic acid | HCID 68762619 | — |
| Solvent | Acetone | HCID 180 | — |
| Product | HCID 68765199 | HCID 68765199 | 38.4% |
Reaction Steps
To a mixture of 2-(3-fluoro-3′-hydroxybiphenyl-4-ylamino)nicotinic acid (1 g, 3.08 mmol) and NaHCO3 (0.5 g, 6.17 mmol) in acetone (20 ml) was added dropwise dimethyl sulphate (0.47 g, 3.70 mmol). The mixture was heated to reflux overnight and then concentrated. Ethyl acetate was added to the crude and washed twice with 4% solution of NaHCO3 and brine. The organic phase was then dried over MgSO4 and concentrated in vacuo to afford 0.4 g of solid beige pure enough for the next synthetic step. Yield=36%
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08691852B2 |
| Source dataset | uspto-grants-2014_04 |
| ORD ID | ord-5e4a390b08ae4f74bb33d8b6a5dfe50a |
| Source note | uspto-grants-2014_04 |