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Triphenylphosphine → n-[(5s)-3-(2-Morpholinoethoxy)-9,10,11-trimethoxy-6,7-dihydro-5h-dibenzo[a,c]cyclohepten-5-yl]acetamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triphenylphosphine | HCID 11776 | — |
| 反応物 | 2-Morpholinoethanol | HCID 61163 | — |
| 反応物 | N-Acetylcolchicinol | HCID 97865 | — |
| 反応物 | Diethyl azodicarboxylate | HCID 5462977 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | n-[(5s)-3-(2-Morpholinoethoxy)-9,10,11-trimethoxy-6,7-dihydro-5h-dibenzo[a,c]cyclohepten-5-yl]acetamide | HCID 9825978 | 37% |
反応手順
DEAD (0.118 g; 0.75 mmol), triphenylphosphine (0.196 g; 0.75 mmol) and 4-(2-hydroxyethyl)morpholine (61 μl; 0.5 mmol) were added to a solution of N-acetyl-colchicinol (0.178 g; 0.5 mmol) in dichloromethane (5 ml) under argon atmosphere. The mixture was stirred at ambient temperature for 6 hours. After evaporation the residue was purified by flash chromatography eluting with a gradient of 2–10% ethanol/dichloromethane to give N-[(5S)-3-(2-morpholinoethoxy)-9,10,11-trimethoxy-6,7-dihydro-5H-dibenzo[a,c]cyclohepten-5-yl]acetamide.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07135502B1 |
| 出典データセット | uspto-grants-2006_11 |
| ORD ID | ord-e3310b1a05b744c28a04a24dbd251ad1 |
| 出典メモ | uspto-grants-2006_11 |