참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | 9-Fluorenylmethyl chloroformate | HCID 34367 | — |
| 반응물 | Methyl 4-Boc-piperazine-2-acetate | HCID 2756816 | — |
| 용매 | Sodium Hydroxide | HCID 14798 | — |
| 생성물 | 1-Fmoc-4-Boc-Piperazine-2-acetic acid | HCID 2756796 | — |
반응 단계
3-Methoxycarbonylmethylpiperazine-1-carboxylic acid tert-butyl ester (6.0 g) was dissolved in TBF (60 ml) and 1N sodium hydroxide solution (60 ml) and stirred at room temperature for 6 hours. The solution was then cooled to 5° C. and adjusted to pH 9-10 by the addition of 10% hydrochloric acid. Nα(9-Fluorenylmethoxycarbonyl chloride (6.05 g) was then added portionwise, maintaining the pH at 9-10 by the addition of 1N NaOH solution. The reaction mixture was stirred at 5° C. for 16 hours. The solution was then adjusted to pH 1 by the addition of 10% hydrochloric acid. The solution was extracted with ethyl acetate (×2), dried (MgSO4) and evaporated. The title compound was obtained as a white foam (9.96 g), mass spectrum (API+) 411 [(M-C4H8)H+], C26H30N2O6 requires 466.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07423052B2 |
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| 출처 데이터셋 | uspto-grants-2008_09 |
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| ORD ID | ord-bd2c7ff1f3a949b6b56b20e3ea0f6d2b |
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| 출처 메모 | uspto-grants-2008_09 |
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