関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 2-Chloroquinazoline | HCID 74054 | — |
| 反応物 | 1-(3-(2-(4-Fluorophenyl)-1,3-dioxolan-2-yl)propyl)piperazine | HCID 2783121 | — |
| 溶媒 | Isopropanol | HCID 3776 | — |
| 生成物 | HCID 13478095 | HCID 13478095 | — |
反応手順
2.25 g 2-Chloroquinazoline, 4.2 g 1-(3-[2-(4-fluorophenyl)-1,3-dioxolan-2-yl]-propyl)piperazine and 2 ml triethylamine in 8 ml isopropanol are stirred and heated 21/2 hours at 80° C. The solvent is then evaporated in vacuo and the residue is taken up in hexane. The hexane solution is treated with charcoal, filtered and concentrated whereby the ketal of the title compound crystallizes out. The resulting precipitate is dissolved in 40 ml aqueous 1N hydrochloric acid. After 1 hour the acidic solution is made alkaline with aqueous ammonia. The resulting precipitate is filtered off and recrystallized from ethyl acetate to give the title compound, m.p. 129°-131° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04588725 |
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| 出典データセット | uspto-grants-1986_05 |
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| ORD ID | ord-08454f3608f04742afd7aee3d64b3985 |
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| 出典メモ | uspto-grants-1986_05 |
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