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Piperidine → 3-({4-[({[(9H-fluoren-9-yl)methoxy]carbonyl}amino)methyl]phenyl}formamido)propanoic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Piperidine | HCID 8082 | — |
| 反応物 | N-Fluorenylmethoxycarbonyl-I2-alanine | HCID 2724630 | — |
| 反応物 | PyBroP | HCID 2733179 | — |
| 反応物 | 4-(((((9H-Fluoren-9-yl)methoxy)carbonyl)amino)methyl)benzoic acid | HCID 2756083 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | N,N-Diethyl-2-propanamine | HCID 521913 | — |
| 生成物 | 3-({4-[({[(9H-fluoren-9-yl)methoxy]carbonyl}amino)methyl]phenyl}formamido)propanoic acid | HCID 22502198 | — |
反応手順
To the above resin bound Fmoc β-alanine was added 500 μL of a 20% solution of piperidine in DMF. Upon shaking for 30 min, the resin was drained and washed with 1 mL DMF containing 1-hydroxybenzotriazole (50 mg/mL) and DMF (2×1 mL). Then 200 μmol 4-[(9H-fluoren-9-ylmethoxycarbonylamino)methyl]benzoic acid (74.2 mg) dissolved in a mixture of 430 μL DMF and 70 μL diethylisopropylamine was added followed by 200 μmol bromo-tris-pyrrolidinophosphonium hexafluorophosphate (PyBrOP, 93 mg) dissolved in 500 μL DMF. The mixture was shaken for 4 hours at 25° C. followed by filtration and washing of the resin with 3×1 mL DMF.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06503949B1 |
| 出典データセット | uspto-grants-2003_01 |
| ORD ID | ord-1298ed63956c4567b4b49f9e236a7d7b |
| 出典メモ | uspto-grants-2003_01 |