HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diisopropylethylamine → 4-(2,3-Dichloro-pyridin-4-yl)-2,2-dimethyl-1-phenyl-piperazine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 2,2-Dimethyl-1-phenylpiperazine | HCID 18628542 | — |
| Reactant | 2,3-Dichloro-4-iodopyridine | HCID 44887038 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | 4-(2,3-Dichloro-pyridin-4-yl)-2,2-dimethyl-1-phenyl-piperazine | HCID 57459618 | — |
Reaction Conditions
| Temperature | 100 °C |
|---|
Reaction Steps
A mixture of D10 (1.083 g, 3.955 mmol), 2,2-dimethyl-1-phenylpiperazine (0.903 g, 4.745 mmol) [C.A.S. 2946-75-0] and DIPEA (1.378 ml, 7.909 mmol) in CH3CN (15 ml) was heated in a sealed tube at 100° C. for 5 days. After cooling, the solvent was concentrated in vacuo. The residue was purified by column chromatography (silica gel; Heptane/EtOAc 100/10 to 80/20 as eluent). The desired fractions were collected and concentrated in vacuo to yield intermediate D55 (0.56 g, 42%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08937060B2 |
| Source dataset | uspto-grants-2015_01 |
| ORD ID | ord-22a7ef7e0921431baace14648baff4b1 |
| Source note | uspto-grants-2015_01 |