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Diisopropylethylamine → HCID 58386517、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 | 7-methoxy-3-(piperidin-4-yl)-4,5-dihydro-1H-benzo[d][1,3]diazepin-2(3H)-one | HCID 18356852 | — |
| 反応物 | (6-Chloropyrimidin-4-yl)-(octahydroindol-1-yl)-methanone | HCID 58386728 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | HCID 58386517 | HCID 58386517 | — |
反応手順
705 mg (2.56 mmol) 7-methoxy-3-piperidin-4-yl-1,3,4,5-tetrahydro-1,3-benzodiazepin-2-one, 680 mg (2.56 mmol) (6-chloro-pyrimidin-4-yl)-(octahydro-indol-1-yl)-methanone and 0.871 mL (5 mmol) DIPEA were stirred in 10 mL DMF for 2 h at RT. The reaction mixture was purified by HPLC. The product-containing fractions were combined and the ACN was eliminated by rotary evaporation. The aqueous phase was made alkaline with 4M NaOH and extracted with EtOAc. The organic phase was dried, filtered and the filtrate was concentrated to dryness by rotary evaporation. The residue was crystallised from a mixture of MeOH and diethyl ether and the solid was suction filtered and dried.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08829006B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-441a4bff0ea9403996c1db01ffb535b0 |
| 出典メモ | uspto-grants-2014_09 |