참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 2-Chloroacrylonitrile | HCID 70198 | — |
| 반응물 | 1,5-Diazabicyclo(5,4,0)undec-5-ene | HCID 314112 | — |
| 반응물 | 1-Amidino-4-phthalimidobutane hydrochloride | HCID 21298870 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 생성물 | 4-Amino-2-(4-phthalimidobutyl)pyrimidine | HCID 20450337 | 42.2% |
반응 단계
A solution of 2-chloroacrylonitrile (1.75 g.) in acetronitrile (10 ml.) was added over 15 minutes to an ice-cooled mixture of 1-amidino-4-phthalimidobutane hydrochloride (5.64 g.), acetonitrile (50 ml.) and 1,5-diazabicyclo[5,4,0]undec-5-ene (6.08 g.). The mixture was stirred for a further two hours and then evaporated to dryness. The residue was treated with water (50 ml.) and the mixture extracted with ethyl acetate (2×50 ml.). The combined ethyl acetate extracts were extracted with N hydrochloric acid (3×30 ml.) and the combined aqueous extracts neutralised with sodium bicarbonate and extracted with ethyl acetate. The ethyl acetate extracts were evaporated to dryness and the residue recrystallised from acetonitrile to give 4-amino-2-(4-phthalimidobutyl)pyrimidine (2.5 g.), m.p. 139°-140°.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04762932 |
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| 출처 데이터셋 | uspto-grants-1988_08 |
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| ORD ID | ord-440b1d3585c8494281a1602658ea97d9 |
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| 출처 메모 | uspto-grants-1988_08 |
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