関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ammonia | HCID 222 | — |
| 反応物 | Methanone, (3-hydroxybenzo[b]thien-2-yl)phenyl- | HCID 4712192 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | HCID 178510717 | HCID 178510717 | — |
反応手順
A mixture of 10.0 gm (0.0393 mol) of 2-benzoylbenzo[b]-thiophen-3-ol, 60 cc of concentrated aqueous ammonia and 250 cc of ethanol was heated for 20 hours at a temperature of 120° C. after introducing 5 bar of ammonia gas into the vessel. After cooling, the mixture was stirred into 1.5 liters of water, the precipitated pale yellow reaction product was filtered off with suction, washed thoroughly several times with 50 cc each of water and dried in the air. 4.23 gm (42% of theory) of yellow crystals, m.p. 121°-122° C., were obtained (after twice recrystallizing from petroleum ether/ethyl acetate 1:1 using activated carbon) and were found to be completely identical with the product obtained in Example 1 based on elemental analysis, IR and UV spectra.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04288437 |
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| 出典データセット | uspto-grants-1981_09 |
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| ORD ID | ord-5d388c9bf3fc411c8812ac7ceb401c01 |
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| 出典メモ | uspto-grants-1981_09 |
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