HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethanol → HCID 73669114, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethanol | HCID 702 | — |
| Reactant | 1,1-Bis(methylthio)-2-nitroethylene | HCID 83623 | — |
| Reactant | HCID 19996035 | HCID 19996035 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 73669114 | HCID 73669114 | 38% |
Reaction Steps
A mixture of N-(6-chloro-3-pyridyl)-1,3-diaminopropane (6.0 g, 0.032 mol)(ex Example 2), 1,1-bis(methylthio)-2-nitroethene (5.34 g, 0.032 mol) and ethanol (100 ml) was heated under reflux for 24 hours. The resulting mixture was evaporated to leave a dark brown oil which was subjected to flash chromatography on a silica column using silica gel, 230 to 400 US mesh (0.062 mm to 0.037 mm), and with 2% w methanol in dichloromethane as eluent. The resulting product was recrystallized from ethanol to give 2-nitromethylene-1-(6-chloro-3-pyridyl)hexahydropyrimidine as a pale yellow solid (3.1 g, 38%), m.p. 202° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05039686 |
| Source dataset | uspto-grants-1991_08 |
| ORD ID | ord-8ad43b322518477fb8684a10d13a7ce2 |
| Source note | uspto-grants-1991_08 |