참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Ammonia | HCID 222 | — |
| 반응물 | Methanol | HCID 887 | — |
| 반응물 | Bromotrimethylsilane | HCID 76113 | — |
| 반응물 | [4-(7-Ethoxymethyl-3-methylxanthin-1-yl)butyl]phosphonate | HCID 19689210 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | Diammonium [4-(7-ethoxymethyl-3-methylxanthin-1-yl)butyl]phosphonate | HCID 86752277 | — |
반응 단계
3.4 ml (0.026 mol) of trimethylsilyl bromide were slowly added dropwise at 0° C., under an argon atmosphere, to a solution of 4.16 g (0.01 mol) of [4-(7-ethoxymethyl-3-methylxanthin-1-yl)butyl]phosphonate in 5 ml of dichloromethane. The solution was stirred at 0° C. for 1 hour and at room temperature for 2 hours. The dichloromethane was then evaporated and the oily residue which remained was dried in a bulb tube in an oil pump vacuum to remove excess trimethylsilyl bromide and ethyl bromide formed. The residue was taken up in a little methanol and treated with 1 ml of concentrated ammonia solution and stirred at room temperature for 2 hours. After evaporating the solvent, the diammonium salt was crystallized from a methanoltdiisopropyl ether mixture.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05728686 |
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| 출처 데이터셋 | uspto-grants-1998_03 |
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| ORD ID | ord-8959e916559b4ac888f77a67d88387d1 |
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| 출처 메모 | uspto-grants-1998_03 |
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