化工社化工社 化学情報印刷レポート · 研究参考用
Nitrogen → 2-Decyl-2,3-dihydrothieno[3,4-b][1,4]dioxine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Nitrogen | HCID 947 | — |
| 反応物 | Toluene | HCID 1140 | — |
| 反応物 | (S)-1,2-Dodecanediol | HCID 2733663 | — |
| 反応物 | 3,4-Dimethoxythiophene | HCID 3613501 | — |
| 触媒 | p-Toluenesulfonic acid monohydrate | HCID 521998 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 2-Decyl-2,3-dihydrothieno[3,4-b][1,4]dioxine | HCID 9856993 | 68.8% |
反応手順
A solution of 3,4-dimethoxythiophene (1.90 g), toluene (30 ml), (S)-1,2-dodecanediol (2.50 g) and p-toluenesulfonic acid monohydrate (100 mg) was heated at 95° C., continuously leading a N2-stream over the solution. After 24 h the reaction mixture was poured into ethyl acetate, washed with NaHCO3 and the organic phase was concentrated. Subsequent filtration over SiO2 using n-hexane/CH2Cl2 (98/2) as eluant resulted in pure product (2.40 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07094865B2 |
| 出典データセット | uspto-grants-2006_08 |
| ORD ID | ord-38c21bccac1c466a9310412c0c189a9d |
| 出典メモ | uspto-grants-2006_08 |