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Diisopropylethylamine → N-Cyclopropyl-N-Methyl-4-{1-[5-Oxo-4-(Tetrahydropyran-4-Ylamino)-6,7-Dihydro-5H-5lambda4-Thieno[3,2-d]Pyrimidin-2-Yl]-Piperidin-4-Yloxy}-Benzamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | (Cyclopropylmethyl)ammonium chloride | HCID 81671 | — |
| 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 | — |
| 反応物 | 4-{1-[5-oxo-4-(tetrahydropyran-4-ylamino)-6,7-dihydro-5H-5lambda4-thieno[3,2-d]pyrimidin-2-yl]-piperidin-4-yloxy}-benzoic acid | HCID 46912845 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | N-Cyclopropyl-N-Methyl-4-{1-[5-Oxo-4-(Tetrahydropyran-4-Ylamino)-6,7-Dihydro-5H-5lambda4-Thieno[3,2-d]Pyrimidin-2-Yl]-Piperidin-4-Yloxy}-Benzamide | HCID 46913023 | — |
反応手順
55 mg of Example 184 (see 40.) are placed in 2 ml dimethylformamide, then 81 l diisopropylethylamine and 53.1 mg O-(7-azabenzotriazol-1-yl-)-N,N,N′,N′-tetramethyluronium hexafluorophosphate (HATU) are added. After 15 min 13.8 mg cyclopropylmethylamine hydrochloride are added. The reaction mixture is stirred at ambient temperature until there is no further reaction and the product is purified directly by preparative HPLC (method B). 30 mg of Example 242 are obtained as a solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08754073B2 |
| 出典データセット | uspto-grants-2014_06 |
| ORD ID | ord-f5998a79fbcc4c73bfae8095fdc14141 |
| 出典メモ | uspto-grants-2014_06 |