HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Hydroxide → X 9121
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | 4-(Chloromethyl)pyridinium chloride | HCID 74570 | — |
| Reactant | HCID 11084280 | HCID 11084280 | — |
| Catalyst | Benzyl triethylammonium chloride | HCID 66133 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | X 9121 | HCID 195376 | — |
Reaction Steps
The title compound was prepared following the procedure of Example 1 from 0.43 g (2.56 mmole) of 4,5-diazafluorene, 0.84 g of 4-picolylchloride hydrochloride, 29.0 mg of benzyltriethylammonium chloride, 3 ml of 50% sodium hydroxide, and 30 ml toluene by reaction at 50° for 6 hrs. The crude product was chromatographed (Ethylacetate/Methanol, 99:1) and recrystallized from isopropyl alcohol. NMR (CDCl3,200 MHz) δ: 3.42(s,4H), 6.52(d,J=5.7 Hz,4H), 7.33(dd,2H), 7.85(d,2H), 8.16(d,J=5.6 Hz,4H), 8.61(d,2H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05300642 |
| Source dataset | uspto-grants-1994_04 |
| ORD ID | ord-a3c4998c98604f6d984250b09860506b |
| Source note | uspto-grants-1994_04 |