関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Cyclopentadiene | HCID 7612 | — |
| 反応物 | 3,5-Dichloroaniline | HCID 12281 | — |
| 反応物 | Glyoxylic acid, monohydrate | HCID 15620607 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 7,9-dichloro-3a,4,5,9b-tetrahydro-3H-cyclopenta[c]quinoline-4-carboxylic acid | HCID 2914772 | — |
反応手順
1.14 g of 3,5-dichloroaniline (10 mmol), 0.97 g of glyoxylic acid hydrate (15 mmol) and 1.40 g of cyclopentadiene (freshly distilled) (30 mmol) were dissolved in 20 ml of acetonitrile in a closable Teflon vessel and heated to 50° C. within one minute in a microwave oven with a power of 800 watts and kept at this temperature for five minutes with further microwave irradiation. The vessel was then placed in ice water, cautiously opened and evaporated in a rotary evaporator. The mass of crystals obtained was washed with hexane and dried. A colourless mass of crystals was obtained in a quantity of 1.95 g (98% of theoretical).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07145011B2 |
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| 出典データセット | uspto-grants-2006_12 |
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| ORD ID | ord-660b88d475be4522bf20f672384a4b5a |
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| 出典メモ | uspto-grants-2006_12 |
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