HuagongsheHuagongshe Chemistry Print Report · For research reference only
Chloromethyl Methyl Ether → HCID 117653471, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Chloromethyl Methyl Ether | HCID 7864 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | HCID 116787092 | HCID 116787092 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 117653471 | HCID 117653471 | — |
Reaction Steps
To a solution of 3-cyano-4-fluoro-N-(pyridazin-3-yl)benzenesulfonamide (Preparation 6, 6.70 g, 24.1 mmol) in DCM (150 mL) at 0° C. was added DIPEA (6.48 mL, 35.18 mmol) followed by chloromethoxymethane (1.46 mL, 25.54 mmol) and the reaction mixture was stirred at room temperature for 2 hours. The reaction mixture was quenched by the addition of 1N NaOH (aq) solution, the organic layer was collected, washed with water, brine, and dried over Na2SO4 before concentrating in vacuo. The residue was purified using silica gel column chromatography eluting with EtOAc:Heptane 1:1 to afford the title compound as a mixture of isomers (3.85 g, 49%) that was used without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09067922B2 |
| Source dataset | uspto-grants-2015_06 |
| ORD ID | ord-87b8218afe1344a3ab48f9a5c1195bd8 |
| Source note | uspto-grants-2015_06 |