HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dichloromethane → HCID 19599740, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | HCID 67574634 | HCID 67574634 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 19599740 | HCID 19599740 | 91.6% |
Reaction Steps
In the same way as that described in Example 2, Step 3 using 2-[(bromoacetyl)(2-(3,4-difluorophenyl)ethyl)amino]ethyl carbamic acid tert-butyl ester (549 mg, 1.3 mmol), trifluoroacetic acid (2.5 mL) and CH2Cl2 (25 mL), followed by K2CO3 (0.36 g, 2.6 mmol) and EtOH (50 mL). The piperazinone (286 mg, 91%) was isolated as a yellow oil. 1H NMR (250 MHz, CDCl3) δ 2.85 (2H, t, J=7.3Hz), 2.99-3.03 (2H, m), 3.17-3.21 (2H, m), 3.52 (2H, s), 3.56 (2H, t, J=7.3Hz), 6.90-7.16 (3H, m). MS (ES+) (241, M+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05998415 |
| Source dataset | uspto-grants-1999_12 |
| ORD ID | ord-3320b7b8651a4e15941e6dea9d9e5589 |
| Source note | uspto-grants-1999_12 |