関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | Sodium Iodide | HCID 5238 | — |
| 反応物 | Chlorotrimethylsilane | HCID 6397 | — |
| 反応物 | 3-Hydroxymethyl-beta-carboline | HCID 5353338 | — |
| 触媒 | Zinc | HCID 23994 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 3-Methyl-9h-pyrido[3,4-b]indole | HCID 13315103 | — |
反応手順
2 g of 3-hydroxymethyl-β-carboline, 3.7 g of sodium iodide and 2.5 ml of chlorotrimethylsilane are stirred in 50 ml of N,N-dimethylformamide at a bath temperature of 35° C. for 4 hours. 3 g of zinc powder and 10 ml of glacial acetic acid are added to the resulting yellow suspension and stirred for another 18 hours at 80° C. The reaction mixture is allowed to clarify on Celite and the filtrate is concentrated under vacuum. The resulting oil is chromatographed on silica gel (methylene chloride/ethanol: 9+1). 0.825 g of 3-methyl-β-carboline with a 255°-256° C. melting point was obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US04731358 |
|---|
| 出典データセット | uspto-grants-1988_03 |
|---|
| ORD ID | ord-221c279277004ba281c77d9f81cbdb36 |
|---|
| 出典メモ | uspto-grants-1988_03 |
|---|
