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HRID 550777作成日:2026年10月26日
Water → 5H-Cyclopenta(d)pyrazolo(1,5-a)pyrimidin-8-amine, 3-(2-chloro-4-methoxyphenyl)-N-(1-ethylpropyl)-6,7-dihydro-2-methyl-
https://huagongshe.com/reaction/550777
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 3-Pentanamine | HCID 12019 | — |
| 反応物 | 8-chloro-2-methyl-3-(2-chloro-4-methoxyphenyl)-6,7-dihydro-5H-cyclopenta[d]pyrazolo[1,5-a]pyrimidine | HCID 11638818 | — |
| 溶媒 | Isopropanol | HCID 3776 | — |
| 溶媒 | Dimethylacetamide | HCID 31374 | — |
| 生成物 | 5H-Cyclopenta(d)pyrazolo(1,5-a)pyrimidin-8-amine, 3-(2-chloro-4-methoxyphenyl)-N-(1-ethylpropyl)-6,7-dihydro-2-methyl- | HCID 9801039 | 85.5% |
反応手順
Under argon gas atmosphere, a mixture of a solution of the compound prepared in Example 5 (177.6 g) in N,N-dimethylacetamide (355 mL) and a solution of triethylamine (103.2 g) and 3-aminopentane (88.9 g) in isopropyl alcohol (178 mL) was stirred for 4 hours at 95 to 105° C. of internal temperature. Water was poured into the reaction solution that was cooled to 70 to 80° C. of internal temperature. The diluted solution was cooled to 50 to 60° C. of internal temperature, and then after the crystal was precipitated, the solution was stirred for 30 minutes. Furthermore, water was poured into the solution, and the diluted solution was stirred for 1 hour at 20 to 30° C. of internal temperature. The precipitated crystal was collected by filtration, and the obtained crystal was dried under reduced pressure for 14 hours or more at about 50° C. to give the crude crystal of the title compound (174 g, (97.4 area %), quantitative value: 85% (two process)).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07947697B1 |
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| 出典データセット | uspto-grants-2011_05 |
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| ORD ID | ord-888d792c538d4e50af3256d6066278ce |
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| 出典メモ | uspto-grants-2011_05 |
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