関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetylacetone | HCID 31261 | — |
| 反応物 | Barium hydroxide, monohydrate | HCID 17749100 | — |
| 反応物 | 1-Butanol propanoic acid | HCID 86646875 | — |
| 触媒 | Tetrabutoxytitanium | HCID 521701 | — |
| 生成物 | Barium propionate | HCID 6096929 | — |
反応手順
2,4 pentanedione (Acac) is degassed by a freeze/pump/thaw method on a Schlenk line over a bed of grade 4A molecular sieves and back filled with argon gas. In a nitrogen-filled drybox, 34.041 g of titanium(IV) n-butoxide (Acros; 0.100 moles) are placed into a 100 ml bottle, and 20.020 g of 2,4 pentanedione (0.200 moles; Aldrich) is then added dropwise and left to stir for 12 hours. In a fumehood, 31.750 g of barium hydroxide hydrate (0.101 moles; Aldrich) is added to a 500 ml volumetric flask. 200 ml of a 50:50 solution of 1-butanol/propanoic acid would then be added and stirred to form barium propanoate. The titanium solution [bis(acetylacetonato)/bis(butoxo)titanium] is then removed from the drybox and added to the volumetric flask containing the barium hydroxide solution. The round bottom flask is rinsed several times with 50:50 1-butanol:propanoic acid solution into the volumetric flask. A 50:50 1-butanol:propanoic acid solution is then added to the 500 ml flask up to the mark, and a stir bar is then added. The solution is stirred for an additional 12 hours.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08088658B2 |
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| 出典データセット | uspto-grants-2012_01 |
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| ORD ID | ord-d95fc86c280a46aa82d7eacc90c68b33 |
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| 出典メモ | uspto-grants-2012_01 |
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