関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Toluene | HCID 1140 | — |
| 反応物 | tert-Butyl hydroperoxide | HCID 6410 | — |
| 反応物 | 2-Chloro-4,5-bis-[(2-methoxyethoxy)-methoxy]-styrol | HCID 18359182 | — |
| 触媒 | Vanadium, oxobis(2,4-pentanedionato-O,O')-, (SP-5-21)- | HCID 5377696 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-Chloro-4,5-bis-[(2-methoxyethoxy)-methoxy]-(1,2-epoxy)-styrol | HCID 18359185 | — |
反応手順
19 g of vanadylacetylacetonate in solution of 50 ml of methylene chloride were cooled to 0° C. and 3.5 ml of terbutyl hydroperoxide in a toluene solution (3M/l) were added over 30 minutes. The mixture was stirred for 20 minutes at 0° C. and 2.63 g of the product of Stage D in solution in 10 ml of methylene chloride were added. The reaction mixture was stirred for 3 hours at ambient temperature and 30 ml of water were added. The organic phase was separated and the solvent was eliminated under reduced pressure. The residue was chromatographed on silica (eluant: methylene chloride-acetone 8-2) to obtain 21.8 g of the expected product with a Rf=0.35 (CH2Cl2 -acetone 8-2).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05712266 |
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| 出典データセット | uspto-grants-1998_01 |
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| ORD ID | ord-f0ae8adaa28a46d2b296fff54604b4df |
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| 出典メモ | uspto-grants-1998_01 |
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