HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylformamide → HCID 46944831, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | Morpholine | HCID 8083 | — |
| Reactant | Oxalyl chloride | HCID 65578 | — |
| Reactant | HCID 66865449 | HCID 66865449 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 46944831 | HCID 46944831 | 90% |
Reaction Steps
4-(3-cyano-1-ethyl-6-methoxy-1H-indol-2-yl)-benzoic acid (50 mg, 0.16 mmol) is suspended in CH2Cl2 (2.2 mL) and catalytic DMF (2 μL). Oxalyl chloride (22 μL, 0.25 mmol) is added. The reaction mixture is stirred at room temperature for 1 hour, at which time full dissolution occurred. This reaction mixture is pipetted dropwise into a vigorously stirring solution of morpholine (1.0 mL) in CH2Cl2 (5 ml). After addition is complete, the reaction mixture is washed with aqueous HCl solution. The organic layer is dried and concentrated. Purification by silica column (1:1 CH2Cl2/EtOAc) yields 1-ethyl-6-methoxy-2-[4-(morpholine-4-carbonyl)-phenyl]-1H-indole-3-carbonitrile (56 mg, 90%) as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07868037B2 |
| Source dataset | uspto-grants-2011_01 |
| ORD ID | ord-e5defa627d6543a5913f209df9c5ac3e |
| Source note | uspto-grants-2011_01 |