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Chloride → N~9~,N~10~-Bis(trimethylsilyl)phenanthrene-9,10-diimine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Chloride | HCID 312 | — |
| 反応物 | 9,10-Phenanthrenedione | HCID 6763 | — |
| 反応物 | Sodium bis(trimethylsilyl)amide | HCID 2724254 | — |
| 反応物 | 1,2-Phenanthrenedione | HCID 3080566 | — |
| 反応物 | Phenanthrenequinone diimine | HCID 86745785 | — |
| 生成物 | N~9~,N~10~-Bis(trimethylsilyl)phenanthrene-9,10-diimine | HCID 71349758 | 37% |
反応手順
Ligand Synthesis. 9,10-Phenanthrenequinone bis((trimethylsilyl)-imine) (silylphi) was synthesized from 9,10-phenanthrenequinone (Aldrich) and sodium bis(trimethylsilyl)amide (Fluka) as described by Tuchtenhagan and Ruhlmann. (11) Important modifications to this synthesis include a reaction temperature of no greater than 65° C. and a final phenanthrenequinone concentration of 0.08 M. Under these conditions, orange crystalline silylphi was obtained in 37% yield and stored under nitrogen. The phenanthrenequinone diimine ligand (phi) was generated and chelated in situ by combining the silylated imine ligand with an ethanolic solution of metal chloride by using a modificaiton of Schlosser's method. (12)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05112974 |
| 出典データセット | uspto-grants-1992_05 |
| ORD ID | ord-0f445a9289244094b55915f4cb38ef55 |
| 出典メモ | uspto-grants-1992_05 |