Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
HRID 432151생성일: 2026년 10월 25일
Sodium hydride → 1-(1,4-dioxaspiro[4.5]dec-8-yl)-3-(4-phenoxyphenyl)-1H-pyrazolo[3,4-d]pyrimidin-4-amine
https://huagongshe.com/reaction/432151
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | 1,4-Dioxaspiro[4.5]decan-8-ol, 8-(4-methylbenzenesulfonate) | HCID 567489 | — |
| 반응물 | HCID 178508717 | HCID 178508717 | — |
| 용매 | Dimethylacetamide | HCID 31374 | — |
| 생성물 | 1-(1,4-dioxaspiro[4.5]dec-8-yl)-3-(4-phenoxyphenyl)-1H-pyrazolo[3,4-d]pyrimidin-4-amine | HCID 22346767 | — |
반응 단계
4-Amino-3-(4-phenoxyphenyl)-1H-pyrazolo[3,4-d]pyrimidine (Compound 15) (4.9 g) in 200 mL dry dimethylacetamide was treated under nitrogen with 60% sodium hydride (2.0 g) and stirred 30 minutes. 1,4-dioxaspiro[4.5]dec-8-yl 4-methyl-1-benzenesulfonate (Intermediate Y) (15 g) was added and the mixture heated at 105° C. for 42 hours. Evaporation in vacuo and treating with water gave solid which was collected and washed well with water then dried in air. The solid was boiled with diethyl ether (6×120 mL) and the filtered solution evaporated. Treatment with acetone gave 1-(1,4-dioxaspiro[4.5]dec-8-yl)-3-(4-phenoxyphenyl)-1H-pyrazolo[3,4-d]pyrimidin-4-ylamine as an off-white solid which was collected and washed with acetone then dried in air m.p. 200-202.5° C. Calculated for C25H25N5O3 C 67.7 H 5.6 N 15.8 Found C 67.6H5.8 N15.4.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06660744B1 |
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| 출처 데이터셋 | uspto-grants-2003_12 |
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| ORD ID | ord-06b4f547c236407ebcd42bb8805c19d0 |
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| 출처 메모 | uspto-grants-2003_12 |
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