化工社化工社 化学情報印刷レポート · 研究参考用
Ethylene Glycol → 1-Boc-4-(2-thienyl)piperazine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethylene Glycol | HCID 174 | — |
| 反応物 | 2-Iodothiophene | HCID 18921 | — |
| 反応物 | Potassium Phosphate, Tribasic | HCID 62657 | — |
| 反応物 | tert-Butyl piperazine-1-carboxylate | HCID 143452 | — |
| 触媒 | Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI) | HCID 24350 | — |
| 溶媒 | Isopropanol | HCID 3776 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 1-Boc-4-(2-thienyl)piperazine | HCID 67343900 | 77% |
反応手順
A mixture of 2-iodothiophene (Aldrich Co., 1.0 g), 1-(tert-butoxycarbonyl)piperazine (Aldrich Co. (hereafter the same), 1.06 g), copper(I) iodide (45 mg), ethylene glycol (530 μl), potassium phosphate (2.02 g) and 2-propanol (5 ml) was heated under reflux for 20 hr. Ethyl acetate was added, and the mixture was filtered through a Celite (trademark) filter. The filtrate was washed 3 times with 28% aqueous ammonia, and then washed with saturated brine. The solvent was evaporated under reduced pressure to give a brown solid. The solid was purified by silica gel column chromatography (elution solvent: ethyl acetate-hexane (7:3)) to give 4-(2-thienyl)piperazine-1-carboxylic acid tert-butyl ester (984 mg, yield 77%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07994196B2 |
| 出典データセット | uspto-grants-2011_08 |
| ORD ID | ord-ffc748b1030f4f6abf2f239762f169db |
| 出典メモ | uspto-grants-2011_08 |