참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | alpha,4-Dichloroanisole | HCID 88801 | — |
| 반응물 | 7-Benzyl-3-methylxanthine | HCID 685630 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 7-Benzyl-1-(4-chlorophenoxymethyl)-3-methylxanthine | HCID 22007319 | — |
반응 단계
2.59 g (19.0 mmol) of potassium carbonate were added at 60° C. to a suspension of 3.0 g (12.0 mmol) of 7-benzyl-3-methylxanthine (prepared according to Example 1a) in 50 ml of dimethylformamide and the mixture was stirred at this temperature for one hour. 2.69 g (15.0 mmol) of 4-chlorophenoxymethyl chloride were then added dropwise and the mixture was stirred at 80° C. for 8 hours. The crude mixture was then filtered, the filtrate was concentrated under reduced pressure, the residue was taken up in dichloromethane, and the solution was washed once with 1 N sodium hydroxide solution and twice with water. The organic phases were dried using magnesium sulfate and concentrated under reduced pressure. The crude product was purified by flash chromatography on a silica gel column, dichloromethane/methanol (19.8/0.2) Yield: 4.15 g (87% of theory); melting point: 96° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06214992B1 |
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| 출처 데이터셋 | uspto-grants-2001_04 |
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| ORD ID | ord-1e17ee0626d943439926e7915051c237 |
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| 출처 메모 | uspto-grants-2001_04 |
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