化工社化工社 化学情報印刷レポート · 研究参考用
Triethylamine → 3-Amino-4-valerylamino thiophene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Valeryl chloride | HCID 61186 | — |
| 反応物 | Thiophene-3,4-diamine | HCID 643216 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 3-Amino-4-valerylamino thiophene | HCID 19370622 | 40.3% |
反応手順
3.06 g of 3,4-diaminothiophene were mixed with 45 ml of methylene chloride and 9 ml of triethylamine and a solution of 3.6 g of valeroyl chloride in 45 ml of methylene chloride was added at a temperature of 20° C. over one hour. The mixture was stirred for 30 minutes, followed by evaporation to dryness. After separation by chromatography (eluant: methanol/methylene chloride 5/95), 3.2 g of the expected monoamide were obtained which was crystallized from 15 ml of a 50/50 mixture of isopropyl ether and cyclohexane. The crystals were separated, washed with this mixture and dried under reduced pressure at 100° C. to obtain 2.14 g of the expected product melting at 110° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05389634 |
| 出典データセット | uspto-grants-1995_02 |
| ORD ID | ord-6e5bfdb6288e4302b1e9238335883240 |
| 出典メモ | uspto-grants-1995_02 |