HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylamine → HCID 19819744, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylamine | HCID 674 | — |
| Reactant | 2-(2-Chloroethyl)-3,4-dihydro-1,4-dimethyl-1H-[1,3,5]triazepino[3,2-a]benzimidazol-5(2H)-one | HCID 19819759 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 19819744 | HCID 19819744 | — |
Reaction Steps
To 90 mL of freshly collected dimethylamine and 10 mL of methanol was added 3.25 g (0.011 mol) of 2-(2-chloroethyl)-3,4-dihydro-1,4-dimethyl-1H-[1,3,5]triazepino[3,2-a]benzimidazol-5(2H)-one. The reaction flask was sealed and left standing at room temperature for 6 days. The dimethylamine was then allowed to evaporate at room temperature and the residue partitioned between 75 mL of 1N NaOH and 75 mL of CH2Cl2. The organic phase was washed with another 50 mL of 1N NaOH. The combined organic layers were dried over Na2SO4, filtered, and concentrated by rotary evaporation. The solid residue was recrystallized from isopropyl ether to give 2.8 g of white analytically pure crystals, mp 91°-95° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05109013 |
| Source dataset | uspto-grants-1992_04 |
| ORD ID | ord-faa5d8b0e54c4a86a33383a9ef172c15 |
| Source note | uspto-grants-1992_04 |