HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phosphorus oxychloride → 6-(Morpholine-4-carbonyl)-1H-indole-3-carbaldehyde
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | (1H-Indol-6-yl)(morpholino)methanone | HCID 39710543 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 6-(Morpholine-4-carbonyl)-1H-indole-3-carbaldehyde | HCID 118666082 | — |
Reaction Steps
A solution of (1H-indol-6-yl)(morpholino)methanone (200 mg, 0.869 mmol, 1.0 eq) in DMF (3.0 ml) was added dropwise at 0° C. to phosphorus oxychloride (0.34 mL, 2.60 mmol, 3.0 eq) in DMF (5.0 mL) under stirring. The mixture was stirred at room temperature for 3 h, then neutralized with saturated sodium hydrogen carbonate solution, diluted with water (20 mL), and extracted with ethyl acetate (2×10 mL). The organic layers were combined, washed with brine (20 mL), dried over sodium sulfate and evaporated. The residue was purified by silica gel column chromatography [100-200 mesh; methanol/dichloromethane=1:9]. White solid. Yield: 100 mg (45% of theory).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09315490B2 |
| Source dataset | uspto-grants-2016_04 |
| ORD ID | ord-984f016470c6402d825e249a38395338 |
| Source note | uspto-grants-2016_04 |