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Water → Zirconium tetrakis(2,2,6,6-tetramethyl-3,5-heptanedionate)
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 2,2,6,6-Tetramethyl-3,5-heptanedione | HCID 70700 | — |
| 反応物 | Zirconium chloride (ZrCl4), (T-4)- | HCID 9856075 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | Zirconium tetrakis(2,2,6,6-tetramethyl-3,5-heptanedionate) | HCID 6287074 | 98.2% |
反応手順
To 177 g of methanol, 43.7 g (0.216 mol) of 2,2,6,6-tetramethyl-3,5-heptanedione of 91% purity was dropwise added with stirring. To the resulting solution, a solution, which had been obtained by dissolving 12.7 g (0.054 mol) of ZrCl4 of 99% purity in 218 g of methanol and cooled to room temperature, was added over a period of about 5 minutes. The reaction was conducted for 1 hour with stirring, and 590 g of water was added over a period of 50 minutes. Then, stirring was performed for 1 hour. The resulting solution was adjusted to pH 6.6 with a 20% NaOH solution. The resulting crystals were collected by centrifugation and then dried. Thus, 43.9 g (yield: 98.2%) of tetrakis(2,2,6,6-tetramethyl-3,5-heptanedionato)zirconium was obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07084306B2 |
| 出典データセット | uspto-grants-2006_08 |
| ORD ID | ord-d031c2a1d4404c0f8c49a7f6d73e8050 |
| 出典メモ | uspto-grants-2006_08 |