HuagongsheHuagongshe Chemistry Print Report · For research reference only
1-(2-Methoxyphenyl)piperazine → HCID 86745195, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1-(2-Methoxyphenyl)piperazine | HCID 1346 | — |
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | 4-(2-Chloroethyl)-3,4-dihydro-2-methylpyrimido[1,6-a]benzimidazol-1(2H)-one | HCID 19989845 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 86745195 | HCID 86745195 | 92.1% |
Reaction Steps
A mixture of 4.0 g (0.015 mol) of 4-(2-chloroethyl)-3,4-dihydro-2-methylpyrimido[1,6-a]benzimidazole-1(2H)-one, 2.93 g (0.015 mol) of 1-(2-methoxyphenyl)piperazine, 9 g of NaHCO3, 0.5 g of Kl, and 30 mL of DMF was heated on a steam cone for 18 h. The reaction mixture was poured into 400 mL of H2O and extracted with 2×100 mL CH2Cl2. The combined organic layers were dried (Na2SO4), filtered and concentrated by rotary evaporation. The resulting oil was purified by preparative HPLC eluting with acetone and using silica gel as the stationary phase. Like fractions were combined and concentrated by rotary evaporation to an oil. The oil was treated with fumaric acid in 2-propanol to give 3.7 g (42%) of the salt, mp 100°-108° C. dec.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05063228 |
| Source dataset | uspto-grants-1991_11 |
| ORD ID | ord-19e9ef3df95b4c999008f407ba6c7c6a |
| Source note | uspto-grants-1991_11 |