HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 23311345, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | (Chloromethyl)cyclopropane | HCID 80013 | — |
| Reactant | HCID 13656118 | HCID 13656118 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 23311345 | HCID 23311345 | 33% |
Reaction Steps
A mixture of 4.0 g (15.8 mmole) of 2-(3-phenyl-2,3-dihydrobenzofuran-3-yl)-N-methylethylamine, 1.54 g (17.1 mmole) cyclopropylmethyl chloride, 6.9 g (50.0 mmole) K2CO3 and 0.2 g KI in 40 ml DMF was warmed to 65° and maintained there for 4 hours. After cooling, the reaction mixture was poured into 400 ml water and extracted with Et2O (3×200 ml). The combined organics were washed with saturated NaCl solution and dried over Na2SO4. After filtration, the solution was stirred with several grams of silica gel and decanted. After adding 1.85 g fumaric acid and stirring for 1 hour, 4.2 g of solid was collected. This material was recrystallized from CH3CN to give 2.2 g (33%) of crystals, m.p. 154°-156°.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04602035 |
| Source dataset | uspto-grants-1986_07 |
| ORD ID | ord-7e68972410be4b87932a527fd807a630 |
| Source note | uspto-grants-1986_07 |