HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dichloromethane → 4-(2-Chloroethyl)-3,4-dihydro-2-methylpyrimido[1,6-a]benzimidazol-1(2H)-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Phosgen toluene | HCID 19083224 | — |
| Reactant | 2-(1-Methyl-3-pyrrolidinyl)-1H-benzimidazole | HCID 19989862 | — |
| Product | 4-(2-Chloroethyl)-3,4-dihydro-2-methylpyrimido[1,6-a]benzimidazol-1(2H)-one | HCID 19989845 | — |
Reaction Steps
A solution of 4 g (0.02 mol) of 2-(1-methyl-3-pyrrolidinyl)-1H-benzimidazole in 100 mL of CH2Cl2 was added dropwise to a solution of 12.5 (0.025 mol) of 20% phosgene/toluene in 30 mL of CH2Cl2. The solution was stirred for 2 h, and 10 g (0.1 mol) of triethylamine was added dropwise. Stirring was continued for 2 h and the solution was extracted with dilute NaOH. The organic layer was dried (Na2SO4) and concentrated. The residue was crystallized twice from isopropyl ether. Yield 1.5 g (28%), mp 88°-91° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05063228 |
| Source dataset | uspto-grants-1991_11 |
| ORD ID | ord-27f19568d9bd4b42a0e6cf1e47ac43b7 |
| Source note | uspto-grants-1991_11 |