참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Flurenol | HCID 10087 | — |
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 반응물 | Proline benzyl ester hydrochloride | HCID 2733413 | — |
| 반응물 | Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1) | HCID 9886157 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 9-hydroxy-9-fluorenylcarbonyl-L-proline benzyl ester | HCID 59038191 | — |
반응 단계
To a solution of 9-hydroxy-9-fluorene carboxylic acid (5.04 g, 22.3 mmol) in N,N-dimethylformamide (30 mL), cooled to 0° C. under nitrogen, was added (O-7-azabenzotriazol-1-y)-1,1,3,3-tetramethyluronium hexafluorophosphate (HATU), (9.32 g, 24.5 mmol), L-proline-benzyl ester hydrochloride (5.93 g, 24.5 mmol), and N,N-diisopropylethylamine (8.5 mL, 48.8 mmol). The mixture was stirred at 0° C. for 3 hours, then concentrated and purified on silica gel (ethyl acetate-hexane, 1:2) to give 9-hydroxy-9-fluorenylcarbonyl-L-proline benzyl ester. HPLC=96%, R.T.=3.7 min; Mass spec.(electrospray) M+1=414.1.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US07144899B2 |
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| 출처 데이터셋 | uspto-grants-2006_12 |
|---|
| ORD ID | ord-d59a48e8a16546be834b83dc63975ec9 |
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| 출처 메모 | uspto-grants-2006_12 |
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