関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 7-Fluoro-4-nitrobenzo-2-oxa-1,3-diazole | HCID 122123 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | (3S,4S,5R,6S)-3-amino-6-(hydroxymethyl)oxane-2,4,5-triol;hydrochloride | HCID 45933886 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-Nbdlg | HCID 87308104 | — |
反応手順
In a brown flask, L-glucosamine hydrochloride (40.0 mg) and NaHCO3 (26.0 mg) were placed and dissolved in water (800 μl). A solution in which 4-fluoro-7-nitro-2,1,3-benzoxadiazole (NBD-F) (92.0 mg) was dissolved in methanol (4.0 ml) was added thereto, and under an argon atmosphere, the resulting mixture was stirred for 2 hours at a bath temperature of 37° C. Thereafter, the mixture was stirred at room temperature for an additional 40 minutes. Methanol was removed by concentration under reduced pressure, and the resulting precipitates (unnecessary substances derived from NBD-F) were removed by filtration. The precipitates were washed with water, and the filtrate and the washing solution were combined, followed by purification by HPLC. A target fraction was collected and lyophilized, whereby a target product was obtained (yield: 48.7 mg, yield ratio: 76%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08986656B2 |
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| 出典データセット | uspto-grants-2015_03 |
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| ORD ID | ord-f6c1e9a5909b4aae9c96477c7f1ebd69 |
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| 出典メモ | uspto-grants-2015_03 |
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