참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Thioacetic acid | HCID 10484 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | HCID 57206022 | HCID 57206022 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | HCID 57041719 | HCID 57041719 | — |
반응 단계
A solution of (2S,4R)-4-methanesulfonyloxy-1-(4-nitrobenzyloxycarbonyl)-2-[2-(4-nitrobenzyloxycarbonylamino)ethyloxymethyl]pyrrolidine (0.90 g) in dimethylformamide (2 ml) was added to a reaction mixture of thioacetic S-acid (0.16 ml) and sodium hydride (62.8% in oil suspension) (0.07 g) in dimethylformamide (9 ml) in a nitrogen stream and the mixture was heated at 70°-75° C. for 6 hours. The mixture was poured into water (100 ml), extracted with ethyl acetate (50 ml×2), dried over magnesium sulfate and concentrated under reduced pressure to give a syrup. The syrup was subjected to a column chromatography on silica gel (20 g) and eluted with chloroform to give (2S,4S)-4-acetylthio-1-(4-nitrobenzyloxycarbonyl)-2-[2-(4-nitrobenzyloxycarbonylamino)ethyloxymethyl]pyrrolidine (0.60 g).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05061804 |
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| 출처 데이터셋 | uspto-grants-1991_10 |
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| ORD ID | ord-1e9525bcb8a1427abf4574e705dd1383 |
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| 출처 메모 | uspto-grants-1991_10 |
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