HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,1-Dichloroethane → HCID 59244836, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,1-Dichloroethane | HCID 6365 | — |
| Reactant | 1-Iodo-3-isocyanatobenzene | HCID 4499000 | — |
| Reactant | Bis-(4-methoxybenzyl)-[5-(2-morpholin-4-yl-6,7-dihydro-5H-pyrrolo[2,3-d]pyrimidin-4-yl)-pyrimidin-2-yl]-amine | HCID 45258862 | — |
| Catalyst | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 59244836 | HCID 59244836 | — |
Reaction Steps
To a dichloroethane solution (10 ml) of bis-(4-methoxy-benzyl)-[5-(2-morpholin-4-yl-6,7-dihydro-5H-pyrrolo[2,3-d]pyrimidin-4-yl)-pyrimidin-2-yl]-amine (540 mg), DMAP (12.2 mg) and 1-iodo-3-isocyanato-benzene (490 mg) were added, followed by refluxing for 17 hours. This was cooled to room temperature, and dichloromethane (40 ml) was added. After washing with saturated aqueous ammonium chloride solution (30 ml), the organic layer was dried over sodium sulfate. After the sodium sulfate was filtered off, the solvent was distilled off under reduced pressure, followed by silica gel column chromatography (hexane/dichloromethane/ethyl acetate=4/4/1 to 1/2/1), to obtain the desired compound as a crude product (404 mg, 51%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08022205B2 |
| Source dataset | uspto-grants-2011_09 |
| ORD ID | ord-8dd169bf21304e31a049bd009d2e54f2 |
| Source note | uspto-grants-2011_09 |