関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | tert-Butyl bromoacetate | HCID 79177 | — |
| 反応物 | 5-Nitro-1-methyl-uracil | HCID 2755734 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | t-Butyl (5-nitro-1-methyl-uracilyl)acetate | HCID 53829665 | 59% |
反応手順
Sodium hydride (0.51 g of a 60% dispersion in mineral oil, 13 mmol) was washed with pentane three times (4 mL each). The compound of Example 109 (2.00 g, 12 mmole) was added portionwise. After the addition was complete, the reaction mixture was stirred for 30 minutes under a nitrogen atmosphere. t-Butyl bromoacetate (1.73 g, 12 mmole) was added in one portion, and the solution was stirred for 3 hours. The reaction mixture was diluted with water (200 mL), and extracted with ethyl acetate (3×50 mL). The combined organic extracts were washed with water (3×50 mL), then brine, dried over magnesium sulfate. The solvent was concentrated, hexanes were added and the solvent was removed in vacuo to afford the title compound (1.97 g) in 59% yield. Rf=0.38 (silica gel, 20% ethyl acetate in dichloromethane.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06342504B1 |
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| 出典データセット | uspto-grants-2002_01 |
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| ORD ID | ord-9de6b4fea52b4c9f91389085fc5c8ade |
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| 出典メモ | uspto-grants-2002_01 |
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