HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → 1,4-bis[(5-bromo-3,4-dihydro-1H-isochromen-1-yl)methyl]piperazine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | Sodium cyanoborohydride | HCID 5003444 | — |
| Reactant | 1-[(5-bromo-3,4-dihydro-1H-isochromen-1-yl)methyl]piperazine | HCID 66643916 | — |
| Reactant | 5-bromo-3,4-dihydro-1H-isochromene-1-carbaldehyde | HCID 77231248 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dichloromethane methanol | HCID 21226129 | — |
| Product | 1,4-bis[(5-bromo-3,4-dihydro-1H-isochromen-1-yl)methyl]piperazine | HCID 68430290 | — |
Reaction Steps
To a solution of 1-[(5-bromo-3,4-dihydro-1H-isochromen-1-yl)methyl]piperazine (160 mg, 0.52 mmol) in DCM/MeOH (1:1, 5 mL) was added DIEA (134 mg, 1.03 mmol), and then mixture was stirred at r.t for 10 min. Then AcOH (62 mg, 1.03 mmol), NaCNBH3 (65 mg, 1.03 mmol) and 5-bromo-3,4-dihydro-1H-isochromene-1-carbaldehyde (125 mg, 0.516 mmol) were added into the mixture. The reaction solution was stirred at ambient temperature overnight. The reaction mixture was added water and extracted with DCM. The organic layer was dried over anhydrous sodium sulfate and concentrated. The residue was purified with prep-TLC to give the product 1,4-bis[(5-bromo-3,4-dihydro-1H-isochromen-1-yl)methyl]piperazine.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08673920B2 |
| Source dataset | uspto-grants-2014_03 |
| ORD ID | ord-c43763d2ad854fdda8799a5744ac4c22 |
| Source note | uspto-grants-2014_03 |