関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 1-Methyl-2-phenylindole | HCID 77095 | — |
| 反応物 | 4,4-Dimethoxy-2-butanone | HCID 228548 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | trans-4-[1-methyl-2-phenyl-1H-indol-3-yl]-3-buten-2-one | HCID 11254370 | 89% |
反応手順
2.07 g of 1-methyl-2-phenyl-1H-indole, 1.32 g of 1,1-dimethoxy-3-butanone and 12 mL of acetic acid were mixed, then, 313 mg of 35 wt % hydrochloric acid was added into the mixture at room temperature, the added mixture was stirred for about 14 hours at the same temperature to cause a reaction. At a time point about 10 minutes after starting of stirring and reaction, blue solid precipitated to render stirring difficult. Therefore, 8 mL of acetic acid was added. After completion of the reaction, 60 mL of water was added dropwise, and the precipitated crystals were filtrated. The crystals were washed with 10 vol % methanol/water, then, dried to obtain 2.44 g of trans-4-[1-methyl-2-phenyl-1H-indol-3-yl]-3-buten-2-one (blue green solid). Yield: 89%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07939674B2 |
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| 出典データセット | uspto-grants-2011_05 |
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| ORD ID | ord-0f619653e2ff42dfa5ec1ae7726cc3f0 |
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| 出典メモ | uspto-grants-2011_05 |
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