関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Tin tetrachloride | HCID 24287 | — |
| 反応物 | ethyl 2-(1H-1,3-benzodiazol-2-yl)acetate | HCID 308071 | — |
| 反応物 | 2-Amino-5-(4-methyl-1-piperazinyl)benzonitrile | HCID 21928519 | — |
| 溶媒 | 1,2-Dichloroethane | HCID 11 | — |
| 生成物 | HCID 178480624 | HCID 178480624 | — |
反応手順
Ethyl 2-benzimidazol-2-ylacetate (1.1 eq) and 2-amino-5-(4-methylpiperazinyl)benzenecarbonitrile (1.0 eq) were dissolved in 1,2-dichloroethane, and then SnCl4 (11 eq) was added. The mixture was heated at reflux overnight. Upon cooling, the mixture was concentrated in vacuo. NaOH (3 M) was added to the solid, and the mixture heated at 80° C. for 0.5 hours. The solid was filtered and washed sequentially with H2O, CH2Cl2, and acetone. LC/MS indicated that the product was present in the acetone layer and the solid. These fractions were combined and purified by silica gel chromatography (5-10% MeOH in CH2Cl2 with 1% Et3N) to give the desired product. LC/MS m/z 375.4 (MH+), Rf 1.65 minutes.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06800760B2 |
|---|
| 出典データセット | uspto-grants-2004_10 |
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| ORD ID | ord-f2e1585b151d40ecb98e8ce46ec367ea |
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| 出典メモ | uspto-grants-2004_10 |
|---|
