HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trifluoroacetic acid → HCID 24960732, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | 4-Methylmorpholine | HCID 7972 | — |
| Reactant | 2-Chloro-4,6-dimethoxy-1,3,5-triazine | HCID 18450 | — |
| Reactant | 4-(4-(5-Amino-pyrimidin-2-ylamino)-benzenesulfonyl)-piperidine-1-carboxylic acid tert-butyl ester | HCID 58748726 | — |
| Reactant | HCID 59652720 | HCID 59652720 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 24960732 | HCID 24960732 | 6% |
Reaction Steps
Intermediate 18 (Example 26) (0.159 g, 0.44 mmol) was combined with 2-chloro-4,6-dimethoxy-1,3,5-triazine (CDMT) (0.093 g, 0.53 mmol) and diluted with DCM (4 mL). This was immediately treated with 4-methyl morpholine (0.10 mL, 0.88 mmol) and allowed to stir at ambient temperature for 1 h. Intermediate 13 (Example 20) (0.20 g, 0.462 mmol) was then added in one portion. Stirring was continued overnight. After 18 h, reaction solvents were removed and resulting crude solids were diluted with DCM (4 mL) and treated with TFA (0.2 mL). After 2 h, reaction solvents were removed and resulting crude solids purified via HPLC to afford the title compound as a white solid (0.017 g, 6%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08030487B2 |
| Source dataset | uspto-grants-2011_10 |
| ORD ID | ord-86e7666142064ddb8975eed95f59aeb1 |
| Source note | uspto-grants-2011_10 |