HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → 4-Amino-N-(4-chlorobenzyl)-1-(7H-pyrrolo[2,3-d]pyrimidin-4-yl)piperidine-4-carboxamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 7H-Pyrrolo(2,3-d)pyrimidine, 4-chloro- | HCID 5356682 | — |
| Reactant | 4-Amino-piperidine-4-carboxylic acid 4-chloro-benzylamide dihydrochloride | HCID 45139621 | — |
| Solvent | 1-Butanol | HCID 263 | — |
| Product | 4-Amino-N-(4-chlorobenzyl)-1-(7H-pyrrolo[2,3-d]pyrimidin-4-yl)piperidine-4-carboxamide | HCID 11675388 | 80% |
Reaction Conditions
| Temperature | 100 °C |
|---|
Reaction Steps
A degassed mixture of 4-amino-piperidine-4-carboxylic acid 4-chloro-benzylamide dihydrochloride (48 mg, 0.13 mmol), 4-chloro-7H-pyrrolo[2,3-d]pyrimidine (21 mg, 0.12 mmol), triethylamine (126 uL, 0.9 mmol) and n-butanol (1.2 mL) was stirred at 100° C. for 18 h. The solvents were removed by evaporation and the crude mixture was first purified on a SCX-II acid resin, eluting with methanol then 2M ammonia/methanol, and then by preparative TLC, eluting with 10% methanol in dichloromethane, to give 4-amino-1-(7H-pyrrolo[2,3-d]pyrimidin-4-yl)-piperidine-4-carboxylic acid 4-chloro-benzylamide (37 mg, 0.096 mmol, 80%). LC-MS (LCT2) m/z 385 [M+H+], Rt 2.84 min.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08796293B2 |
| Source dataset | uspto-grants-2014_08 |
| ORD ID | ord-42c022b1704f4dd8a6eaf192ce9ae4f5 |
| Source note | uspto-grants-2014_08 |