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Diisopropylethylamine → 6-Propoxy-5-pyrrolidin-1-yl-pyrazine-2-carboxylic acid ((S)-1-hydroxymethyl-3-methyl-butyl)-amide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | L-Leucinol | HCID 111307 | — |
| 反応物 | O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborate | HCID 2733207 | — |
| 反応物 | 6-Propoxy-5-pyrrolidin-1-yl-pyrazine-2-carboxylic acid | HCID 68567445 | — |
| 溶媒 | Formic Acid | HCID 284 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 6-Propoxy-5-pyrrolidin-1-yl-pyrazine-2-carboxylic acid ((S)-1-hydroxymethyl-3-methyl-butyl)-amide | HCID 24831258 | 24% |
反応手順
A mixture of 6 mg (0.024 mmol) 6-propoxy-5-pyrrolidin-1-yl-pyrazine-2-carboxylic acid, 9.3 mg (0.029 mmol) TBTU, 9.3 mg (0.072 mmol) DIPEA and 4.2 mg (0.036 mmol) (S)-2-amino-4-methyl-pentan-1-ol (commercially available) in 1 mL DMF was shaken at room temperature for 16 h. After addition of formic acid the mixture was subjected to purification by preparative HPLC on reversed phase eluting with a gradient formed from acetonitrile, water and formic acid. The combined product fractions were evaporated to yield 2 mg (24%) of the title compound. m/z (ES+): 351.5 (M+H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07691863B2 |
| 出典データセット | uspto-grants-2010_04 |
| ORD ID | ord-13572c0ed70f480daa3350330e68eace |
| 出典メモ | uspto-grants-2010_04 |