関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | L-(+)-Cysteine | HCID 5862 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | Xanthydrol | HCID 72861 | — |
| 溶媒 | Trifluoroacetic acid | HCID 6422 | — |
| 溶媒 | 1,2-Dimethoxyethane | HCID 8071 | — |
| 生成物 | S-(9H-Xanthen-9-yl)cysteine | HCID 10566205 | 86.3% |
反応手順
A sample of 0.61 g of cysteine (5 mmole) was suspended in 100 ml of 1,2-dimethoxyethane and 2 ml of TFA. The suspension was stirred under nitrogen gas at room temperature until the solution became clear. To this clear solution was added 1 g of 9H-xanthen-9-ol (5.1 mmole) in one portion. The reaction mixture was stirred at room temperature for 30 minutes and was then neutralized to pH 7 by the addition of a saturated aqueous Na2CO3 solution. The mixture was then concentrated by rotary evaporation. The residue was diluted with 50 ml of water. The aqueous solution was treated with 10% aqueous citric acid solution to adjust the pH to 6. The mixture was stirred at room temperature for 1 hr. The resultant white solid was collected by filtration and was washed with 3×10 ml of water and 3×10 ml of ethyl acetate. The product was dried to yield 1.30 g of product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07745392B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-946029af8d8640cf8e47831f71bc71c6 |
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| 出典メモ | uspto-grants-2010_06 |
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