HuagongsheHuagongshe Chemistry Print Report · For research reference only
3,5-Dimethyl-4-hydroxybenzonitrile → HCID 57848883, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 3,5-Dimethyl-4-hydroxybenzonitrile | HCID 20176 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 2,4-Dichlorothieno[3,2-d]pyrimidine | HCID 12712832 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | N-methyl-2-pyrrolidone | HCID 13387 | — |
| Product | HCID 57848883 | HCID 57848883 | 315% |
Reaction Steps
A stirred suspension of NaH (29.7 mg, 0.74 mmol) in dry NMP (3.5 mL) was added 4-hydroxy-3,5-dimethylbenzonitrile (108.2 mg, 0.74 mmol) and stirred at room temperature for 30 min under Argon. The reaction mixture was added to a solution of 2,4-dichlorothieno[3,2-d]pyrimidine (39.6 mg, 0.19 mmol) in dry NMP (4 mL) and heated at 50° C. for 5 h. The resulting mixture was diluted with water and washed with EtOAc. The combined organic layers were washed with water, brine, dried over Na2SO4, filtered and concentrated in vacuo. The crude product was purified by column chromatography, eluting with hexanes/ethyl acetate (4:1) to give the product as a white solid (189 mg, 81%):
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07595324B2 |
| Source dataset | uspto-grants-2009_09 |
| ORD ID | ord-f263cc303b2a489d9a78805c788aa37a |
| Source note | uspto-grants-2009_09 |