HuagongsheHuagongshe Chemistry Print Report · For research reference only
Citric Acid → HCID 58016880, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Citric Acid | HCID 311 | — |
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Neopentyl glycol | HCID 31344 | — |
| Reactant | 4-Chloro-5-(4-methoxyphenyl)-6-phenylfuro[2,3-d]pyrimidine | HCID 58016815 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 58016880 | HCID 58016880 | — |
Reaction Steps
Put 1.546 g (14.85 mmol) 2,2-dimethylpropane-1,3-diol in 30 ml THF. Add 833 mg (7.42 mmol) potassium tert.-butylate and stir for a further 15 min at RT. Then cool to 0° C. and add a solution of 1.00 g (2.97 mmol) 4-chloro-5-(4-methoxyphenyl)-6-phenylfuro[2,3-d]pyrimidine in 15 ml THF dropwise over a time of 30 min. Leave to return to RT and stir for a further 30 min at RT. Then add dichloromethane and water, acidify with 10% citric acid solution and separate the phases. Extract the aqueous phase once with dichloromethane. Combine the organic phases and wash once with satd. sodium chloride solution, dry over magnesium sulphate and concentrate by evaporation. 1.20 g (99.9% of theor.) of the target compound is obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08183246B2 |
| Source dataset | uspto-grants-2012_05 |
| ORD ID | ord-5850fff812ba4e12b50fd377360ee2c7 |
| Source note | uspto-grants-2012_05 |