참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 1,2-Dimethylhydrazine dihydrochloride | HCID 9380 | — |
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 반응물 | 5-Benzyloxy-2-methanesulfonyl-1-methoxycarbonylmethyl-6-oxo-1,6-dihydro-pyrimidine-4-carboxylic acid ethyl ester | HCID 18442531 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | HCID 18442536 | HCID 18442536 | 69% |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US07192948B2 |
|---|
| 출처 데이터셋 | uspto-grants-2007_03 |
|---|
| ORD ID | ord-c4ad857185174b728b2b069bd279f61c |
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| 출처 메모 | uspto-grants-2007_03 |
|---|
