HuagongsheHuagongshe Chemistry Print Report · For research reference only
Benzoyl chloride → HCID 59592965, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Benzoyl chloride | HCID 7412 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 4-(4,4,5,5-Tetramethyl-1,3,2-dioxaborolan-2-yl)-1H-indazole | HCID 45480186 | — |
| Reactant | HCID 59592865 | HCID 59592865 | — |
| Solvent | Hydrochloric Acid | HCID 313 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 59592965 | HCID 59592965 | — |
Reaction Steps
To a solution of 2-(2-chloro-4-morpholinothieno[3,2-d]pyrimidin-6-yl)propan-2-amine (1.1 g, 3.5 mmol) in CH2Cl2 (50 mL) was added Et3N (0.6 mL, 4.9 mmol) and benzoyl chloride (0.6 mL, 4.2 mmol). The resulting mixture stirred at room temperature overnight. The reaction was diluted with 1 M HCl and extracted with DCM, dried over MgSO4, and concentrated in vacuo. The crude material was purified by silica gel chromatography (0-50% EtOAc in hexane). A portion (0.65 mmol) of the crude material was utilized in a Suzuki coupling using General Procedure A with 4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1H-indazole 7 to provide 388 after reverse phase HPLC purification (133 mg). MS (Q1) 499 (M)+
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08450315B2 |
| Source dataset | uspto-grants-2013_05 |
| ORD ID | ord-a6eccc22f28f420fae5637751b3974dd |
| Source note | uspto-grants-2013_05 |