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Diisopropylethylamine → HCID 44561082、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 | 4-(Methylamino)tetrahydro-2H-pyran | HCID 6991950 | — |
| 反応物 | ethyl 4-chloro-1-ethyl-1H-pyrazolo[3,4-b]pyridine-5-carboxylate | HCID 10491120 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | HCID 44561082 | HCID 44561082 | 76.5% |
反応手順
Intermediate 1 (1.2 g, 4.76 mmol), Intermediate 50 (0.79 g, 5.2 mmol) and diisopropylethylamine (4 ml, 24 mmol) in MeCN (8 ml) was heated at 70° C. for 24 hours. The solvent was removed in vacuo and the residue partitioned between DCM and water. The organic phase was concentrated in vacuo and the residue chromatographed on silica (50 g) eluting with cyclohexane:ethyl acetate (2:1 followed by 1:1 then 1:2). Appropriate fractions were combined and evaporated to give Intermediate 51 as a brown oil (1.21 g). LCMS showed MH+=334; TRET=2.61 min.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07528148B2 |
| 出典データセット | uspto-grants-2009_05 |
| ORD ID | ord-6bb30160f5c549bca1f5b8d0dc14c418 |
| 出典メモ | uspto-grants-2009_05 |