関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Chloride | HCID 5234 | — |
| 反応物 | Allyl chloride | HCID 7850 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 2-Oxazoleethanol, 4,5-dihydro-beta-methyl- | HCID 114555 | — |
| 反応物 | t-Bu4NHSO4 | HCID 9927882 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Heptane | HCID 8900 | — |
| 生成物 | 2-{1-[(Prop-2-en-1-yl)oxy]propan-2-yl}-4,5-dihydro-1,3-oxazole | HCID 14028676 | 99% |
反応手順
In a three-neck round bottom flask, 24 g allylchloride (0.31 mole), 60 g 2-(3-hydroxy-2-propyl)-2-oxazoline (0.47 mole), 10 g of heptane, and 3.7 g (t-Bu)4NHSO4 phase transfer catalyst in 150 g tetrahydrofuran (THF) are added as the organic phase. The aqueous phase is 93 g NaOH solution prepared by dissolving 50 wt % NaOH into H2O saturated with NaCl. The solution is agitated vigorously by a mechanical stirrer. Reaction is conducted at 40° C. for 3.5 hours. Conversion is over 90% according to GC analysis of crude product. After the reaction, the aqueous layer is decanted and the organic layer is extracted four times with H2O saturated with NaCl. Tetrahydrofuran solvent is stripped off by a rotary evaporator. The remaining solution is filtered and dried over 3 Å molecular sieve. A pure monomer (99%) is obtained by distillation (0.12 mm/31° C.). The structure is identified by NMR and IR analysis.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US04709039 |
|---|
| 出典データセット | uspto-grants-1987_11 |
|---|
| ORD ID | ord-8c40477f8f3e4d22a22a90531e97a99b |
|---|
| 出典メモ | uspto-grants-1987_11 |
|---|