HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 66674649, compound → HCID 24938255, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 66674649 | HCID 66674649 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | Ammonia | HCID 222 | 7% |
| Product | HCID 24938255 | HCID 24938255 | 8.2% |
Reaction Steps
Dissolve the [6-fluoro-4-(2-{2-[2-(2-oxo-imidazolidin-1-yl)-ethylamino]-pyrimidin-4-yl}-benzo[b]thiophen-7-yl)-pyridin-3-yl]-carbamic acid tert-butyl ester into dichloromethane and adsorb onto silica gel (10 g) via concentration in vacuo. Dry under high vacuum for 24 hours. Place silica gel into a round bottom flask and heat in a temperature controlled oil bath to 98-99° C. while under high vacuum for 2 hours. Cool to room temperature. Extract product from silica gel with 10% 7 N ammonia in methanol/90% dichloromethane. Concentrate in vacuo. Chromatograph on silica eluting with a gradient of 100% dichloromethane to 7% 2 N ammonia in methanol/93% dichloromethane to afford the title compound (65.2 mg, 8.2%). MS (ES) m/z 450 [M+1]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08101628B2 |
| Source dataset | uspto-grants-2012_01 |
| ORD ID | ord-4dfc7ad1c9dc400e9cb57fea8051b1a2 |
| Source note | uspto-grants-2012_01 |