HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 59593276, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | Acetylacetone | HCID 31261 | — |
| Reactant | tert-Butyl 3-(chloromethyl)-1H-pyrrolo[2,3-b]pyridine-1-carboxylate | HCID 21463021 | — |
| Solvent | Dimethyl Sulfoxide | HCID 679 | — |
| Product | HCID 59593276 | HCID 59593276 | — |
Reaction Steps
To acetylacetone (0.563 g, 5.62 mmol) in dimethyl sulfoxide (29.0 mL) was added sodium hydride (0.225 g, 60% in mineral oil, 5.62 mmol). After 20 minutes, 3-chloromethyl-pyrrolo[2,3-b]pyridine-1-carboxylic acid tert-butyl ester (512, 1.00 g, 3.75 mmol) was added to the reaction. The reaction was stirred at room temperature for 2 hours. The reaction was poured into water and extracted with ethyl acetate. The organic layer was dried over anhydrous sodium sulfate and filtered. The filtrate was concentrated and purified by silica gel column chromatography eluting with 40% ethyl acetate in hexane to give a colorless oil (513, 0.59 g, 48.0%). MS (ESI) [M+H+]+=331.4.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08722702B2 |
| Source dataset | uspto-grants-2014_05 |
| ORD ID | ord-c907349768824561b829f4a6ff02401d |
| Source note | uspto-grants-2014_05 |