関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylamine | HCID 674 | — |
| 反応物 | 1,4-Diazabicyclo(2.2.2)octane--trimethylalumane (1/2) | HCID 16688366 | — |
| 反応物 | 7-(4-Benzyl-piperazin-1-yl)-benzofuran-2-carboxylic acid ethyl ester | HCID 59636745 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Sodium chloride; water | HCID 57417360 | — |
| 生成物 | 7-(4-benzylpiperazin-1-yl)-N,N-dimethylbenzofuran-2-carboxamide | HCID 59636770 | 87.7% |
反応手順
7-(4-Benzyl-piperazin-1-yl)-benzofuran-2-carboxylic acid ethyl ester (1.0 g, 2.74 mmol) and DABAL-Me3 (0.56 g, 2.20 mmol) were mixed in tetrahydrofuran (5 mL). Dimethylamine (2M in THF) (2.2 mL, 4.39 mmol) was added and the mixture was heated by microwave irradiation to 120° C. for 15 min. Brine was added and the mixture was extracted with dichloromethane, dried over Na2SO4, filtered and the solvent removed by rotary evaporation. The product was purified by flash chromatography (SiO2; DCM/MeOH; gradient 0-2%) giving 7-(4-benzylpiperazin-1-yl)-N,N-dimethylbenzofuran-2-carboxamide (0.70 g, 1.93 mmol) in 70% yield.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08859534B2 |
|---|
| 出典データセット | uspto-grants-2014_10 |
|---|
| ORD ID | ord-fad5ab25af9f4a149521755b80ec1b68 |
|---|
| 出典メモ | uspto-grants-2014_10 |
|---|
