関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Phenyl ethenesulfonate | HCID 564920 | — |
| 反応物 | 2-((1,1-Dimethylethyl)imino)-N,N-diethylhexahydro-1,3-dimethyl-2lambda5-1,3,2-diazaphosphorin-2-amine | HCID 3513851 | — |
| 反応物 | 7H-indolo[2,1-a][2]benzazepine-10-carboxylic acid | HCID 66639679 | — |
| 反応物 | 3-cyclohexyl-2-(2-formyl-4-methoxyphenyl)-1H-indole-6-carboxylate | HCID 86760772 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 1-Methyl-4-(vinylsulfonyl)piperazine | HCID 59837580 | 52% |
反応手順
7H-Indolo[2,1-a][2]benzazepine-10-carboxylic acid, 13-cyclohexyl-3-methoxy-6-(phenoxysulfonyl)-,1,1-dimethylethyl ester. To a solution of tbutyl 3-cyclohexyl-2-(2-formyl-4-methoxyphenyl)-1H-indole-6-carboxylate (4.40 g, 11.2 mmol) in dioxane (30.0 mL) and BEMP (4.88 mL, 16.9 mmol) was added phenyl vinylsulfonate (4.14 g, 22.5 mmol). The resulting mixture was stirred at 22° C. for 1 hr and then at 110° C. in a sealed tube in a microwave for 15 min. The resulting mixture was concentrated under reduced pressure. Silica gel chromatography (1:1 EtOAc:hexanes) of the concentrate afforded the title compound (3.49 g, 52%) as a yellow oil. MS m/z 600 (MH+), ret time 3.11 min, column B, 4 minute gradient, flow rate 4 mL/min.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07456167B2 |
|---|
| 出典データセット | uspto-grants-2008_11 |
|---|
| ORD ID | ord-a280fb2a30fa4f82a578fd6d00456f67 |
|---|
| 出典メモ | uspto-grants-2008_11 |
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