HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → 4-((4-Chlorobenzyloxy)methyl)-1-(7H-pyrrolo[2,3-d]pyrimidin-4-yl)piperidin-4-amine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 7H-Pyrrolo(2,3-d)pyrimidine, 4-chloro- | HCID 5356682 | — |
| Reactant | 4-(4-Chloro-benzyloxymethyl)-piperidin-4-ylamine dihydrochloride | HCID 45139439 | — |
| Solvent | 1-Butanol | HCID 263 | — |
| Product | 4-((4-Chlorobenzyloxy)methyl)-1-(7H-pyrrolo[2,3-d]pyrimidin-4-yl)piperidin-4-amine | HCID 11703456 | 78.6% |
Reaction Conditions
| Temperature | 100 °C |
|---|
Reaction Steps
A degassed mixture of 4-(4-chloro-benzyloxymethyl)-piperidin-4-ylamine dihydrochloride (9.2 mg, 0.028 mmol), 4-chloro-7H-pyrrolo[2,3-d]pyrimidine (5.9 mg, 0.035 mmol), triethylamine (36 uL, 0.2 mmol) and n-butanol (0.35 mL) was stirred at 100° C. for 17 h. The solvents were removed by evaporation. The crude mixture was purified on an 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-(4-chloro-benzyloxymethyl)-1-(7H-pyrrolo[2,3-d]pyrimidin-4-yl)-piperidin-4-ylamine (8.2 mg, 0.022 mmol, 78%). LC-MS (LCT2) m/z 372 [M+H+], Rt 3.19 min.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08796293B2 |
| Source dataset | uspto-grants-2014_08 |
| ORD ID | ord-b02855824c944619ab3e62d02e1c2ccf |
| Source note | uspto-grants-2014_08 |