HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylformamide → HCID 22672848, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | Oxalyl chloride | HCID 65578 | — |
| Reactant | Cesium | HCID 5354618 | — |
| Reactant | HCID 22672852 | HCID 22672852 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 22672848 | HCID 22672848 | — |
Reaction Steps
A suspension of the title D compound, 2-benzyloxy-5-(2,6-dimethyl-4-nitrophenoxy)-benzenesulfonic acid, cesium salt (9.9 g, 20 mmol) in 200 mL of CH2Cl2 is treated with DMF (3.1 mL, 40 mmol), then oxalyl chloride (3.5 mL, 40 mmol) is added over 30 min at RT. The reaction mixture is stirred for 1 h further, then diluted with Et2O (200 mL) and washed with water and brine, dried over anhydrous sodium sulfate (Na2SO4) and concentrated. The product is washed with Et2O (5 mL) and dried in vacuo to afford 2-benzyloxy-5-(2,6-dimethyl-4-nitro-phenoxy)benzenesulfonyl chloride: NMR (CDCl3) 2.24 (s, 6H), 5.31 (s, 2H), 7.02 (dd, 1H, J=8.7, 3.8), 7.10 (d, 1H, J=8.7), 7.32-7.47 (m, 4H), 7.52 (d, 2H, J=7.5), 8.05 (s, 2H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06790978B2 |
| Source dataset | uspto-grants-2004_09 |
| ORD ID | ord-24a198c8dd11462db99d2b8ec198a7f5 |
| Source note | uspto-grants-2004_09 |