関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Flurenol | HCID 10087 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | Proline benzyl ester hydrochloride | HCID 2733413 | — |
| 反応物 | Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1) | HCID 9886157 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 9-hydroxy-9-fluorenylcarbonyl-L-proline benzyl ester | HCID 59038191 | — |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07144899B2 |
|---|
| 出典データセット | uspto-grants-2006_12 |
|---|
| ORD ID | ord-d59a48e8a16546be834b83dc63975ec9 |
|---|
| 出典メモ | uspto-grants-2006_12 |
|---|
