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Diisopropylethylamine → HCID 86603081、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborate | HCID 2733207 | — |
| 反応物 | 6-fluoro-1H-indole-7-carboxylic Acid | HCID 11708161 | — |
| 反応物 | HCID 68882968 | HCID 68882968 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | HCID 86603081 | HCID 86603081 | 85% |
反応手順
To a solution of 50 mg (0.28 mmol) of 6-fluoro-1H-indole-7-carboxylic acid and 90 mg of TBTU (0.28 mmol) in 4 ml DMF, were added 0.24 ml (1.4 mmol) of N,N-diisopropylethyl amine. After stirring for 5 min at rt, 180 mg (0.28 mmol) acid of (4-tert-butyl-benzyl)-[2-(3,4-difluoro-phenyl)-ethyl]-amine were added. After stirring for 17 h at rt, the reaction mixture was diluted with 50 ml water and extracted with 2×50 ml EtOAc. The combined organic phases were washed with water and brine, dried with magnesium sulfate, filtered and concentrated in vacuo. The residue was purified by column chromatography (9 g silica gel; EtOAc/heptane 1:4) to give 85 mg light yellow foam (85%). MS 464.1 (M)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07259183B2 |
| 出典データセット | uspto-grants-2007_08 |
| ORD ID | ord-66fa25f7b5e1453a849a8e2d23a3c5a7 |
| 出典メモ | uspto-grants-2007_08 |