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Water → 2-(4-Chlorophenyl)-2-(4-nitrophenyl)-1,3-dioxolane
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 | p-Toluenesulfonic acid | HCID 6101 | — |
| 反応物 | 4-Chloro-4'-nitrobenzophenone | HCID 347771 | — |
| 溶媒 | Ethylene Glycol | HCID 174 | — |
| 生成物 | 2-(4-Chlorophenyl)-2-(4-nitrophenyl)-1,3-dioxolane | HCID 15489626 | 91% |
反応手順
Toluene (1900 ml) was stirred in a round-bottom flask (51) using a water separator. (4-Chlorophenyl)(4-nitrophenyl)methanone (250 g) was added portionwise. p-Toluene-sulfonic acid (54.5 g) was added portionwise. Ethylene glycol (237.5 g) was poured out into the mixture. The mixture was stirred and refluxed for 48 hours. The solvent was evaporated. The residue was dissolved into ethyl acetate (5 l) and washed twice with a K2CO3 10% solution. The organic layer was separated, dried (MgSO4), filtered and the solvent was evaporated. The residue was stirred in DIPE, filtered off and dried (vacuum, 40° C., 24 hours), yielding 265 g (91%) of 2-(4-chlorophenyl)-2-(4-nitrophenyl)-1,3-dioxolane (interm. 5-a).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06169096A |
| 出典データセット | uspto-grants-2001_01 |
| ORD ID | ord-f1a653b03e0c40d1ae8146d7d9fbdcab |
| 出典メモ | uspto-grants-2001_01 |