HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 57990268, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Cyanoacetic acid | HCID 9740 | — |
| Reactant | Oxalyl chloride | HCID 65578 | — |
| Reactant | HCID 57990316 | HCID 57990316 | — |
| Catalyst | Dichloromethane | HCID 6344 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 57990268 | HCID 57990268 | 46.9% |
Reaction Steps
To a suspension of cyanoacetic acid (46 mg, 0.54 mmol) in CH2Cl2 (1 mL) (containing 2 drops of DMF), oxalyl chloride (0.047 mL, 0.54 mmol) was added. The mixture was stirred at room temperature for 40 min. To the above solution cooled in an ice bath, a solution of 4-(4-(piperidin-3-ylamino)-7H-pyrrolo[2,3-d]pyrimidin-2-ylamino)benzamide (18 mg, 0.051 mmol) and TEA (0.250 mL, 1.80 mmol) in DMF (2 mL) was added. The mixture was stirred for 2 h. Water was added. CH2Cl2 was removed in vacuo. The residue was purified by HPLC to give the titled compound (10 mg). MS 419.3 (M+H); UV 201.6, 311.9 nm.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08258144B2 |
| Source dataset | uspto-grants-2012_09 |
| ORD ID | ord-9c9a537d8ca747a796e8e3aeb9ff6eba |
| Source note | uspto-grants-2012_09 |