HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylformamide → HCID 15896094, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | Oxalyl chloride | HCID 65578 | — |
| Reactant | HCID 15896092 | HCID 15896092 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 15896094 | HCID 15896094 | — |
Reaction Steps
To a solution of the carboxylic acid from Example 33 (0.080 g, 0.20 mmol) under a nitrogen atmosphere in dichloromethane (25 ml) at 0° C. were added DMF (20 □l) and oxalyl chloride (31 mg, 0.24 mmol). The mixture was stirred at 0° C. to room temperature for 2 h and then concentrated in vacuo. The residue was dissolved in methanol (4 ml) and dichloromethane (16 ml) and the mixture stirred at room temperature for 16 h. The mixture was then washed with 1M KHSO4 (3 times), saturated sodium bicarbonate solution (3 times) and brine, dried over Na2SO4, and concentrated in vacuo. The residue was purified by flash chromatography on silica (eluant dichloromethane:methanol 96:4) to give a white solid; yield 0.049 g (60%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07176195B2 |
| Source dataset | uspto-grants-2007_02 |
| ORD ID | ord-851df4d5ef5349ad8f26bc38e78d7acf |
| Source note | uspto-grants-2007_02 |