関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1,2-Dimethylhydrazine dihydrochloride | HCID 9380 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 5-Benzyloxy-2-methanesulfonyl-1-methoxycarbonylmethyl-6-oxo-1,6-dihydro-pyrimidine-4-carboxylic acid ethyl ester | HCID 18442531 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | HCID 18442536 | HCID 18442536 | 69% |
反応手順
A mixture of intermediate 3, ethyl 5-benzyloxy-1-(methoxycarbonylmethyl)-2-(methylsulfonyl)-6-oxo-1,6-dihydropyrimidine-4-carboxylate, (0.487 g, 1.15 mmol) in N,N-dimethylformamide (25 ml) was treated with 1,2-dimethylhydrazine dihydrochloride (1.56 g, 11.7 mmol) followed by N,N-diisopropylethylamine (4.1 ml, 11.7 mmol) and the resulting mixture stirred at 22° C. for 4 h. The solvent was then removed in vacuo and the residue diluted with ethyl acetate, washed successively with saturated sodium bicarbonate and brine then dried over anhydrous magnesium sulfate. Evaporation of the solvent followed by chromatography on silica gel (elution with a gradient of ethyl acetate 0–50% in toluene) gave 0.294 g (69% yield) of the title ester as a clear syrup.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07192948B2 |
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| 出典データセット | uspto-grants-2007_03 |
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| ORD ID | ord-c4ad857185174b728b2b069bd279f61c |
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| 出典メモ | uspto-grants-2007_03 |
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