関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | Methyl 6-aminohexanoate hydrochloride | HCID 11499324 | — |
| 反応物 | 4-Chloro-6-phenylfuro[2,3-d]pyrimidine | HCID 57946488 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Methyl 6-[(6-phenylfuro[2,3-d]pyrimidin-4-yl)amino]hexanoate | HCID 25123737 | — |
反応手順
Heat 2.0 g (8.67 mmol) 4-chloro-6-phenylfuro[2,3-d]pyrimidine and 6.04 ml (34.7 mmol) DIEA in 5 ml DMF to 160° C. Add 3.15 g (17.34 mmol) 6-aminohexanoic acid methyl ester hydrochloride and stir for 4 h at 160° C. After cooling, add the mixture to ice water and extract three times with ethyl acetate. Combine the organic phases and wash with saturated ammonium chloride solution, dry over magnesium sulphate and concentrate under vacuum. Add methanol to the oil residue. Filter off the precipitated solid with suction, wash with methanol again and dry the solid at high vacuum. 1.85 g (57.2% of theor.) of the target compound is obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08183246B2 |
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| 出典データセット | uspto-grants-2012_05 |
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| ORD ID | ord-5cdc9941b0684131bd89d6c7c9fe9ad1 |
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| 出典メモ | uspto-grants-2012_05 |
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