関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 3-Chloro-6-phenylpyridazine | HCID 88515 | — |
| 反応物 | (1S,4S)-2-Boc-2,5-diazabicyclo[2.2.1]heptane | HCID 11521263 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | HCID 15462093 | HCID 15462093 | 49.2% |
反応手順
Triethylamine (20 mL) was added to a suspension of t-butyl (S,S)-2,5-diazabicyclo[2.2.1]heptane-2-carboxylate (3.43 g, 17.3 mmol, Aldrich Chemical Company) and 3-chloro-6-phenylpyridazine (3.30 g, 17.3 mmol, Aldrich Chemical Company) in toluene (50 mL) and the mixture was heated under nitrogen at 100° C. for 7 days. The dark mixture was cooled to room temperature, and the resulting precipitate was isolated by filtration, washed with toluene (15 mL) and dried under vacuum to provide the title compound as an off-white solid (3.00 g). The filtrate was concentrated and the residue wa purified by column chromatography on silica gel, eluting with ethyl acetate, to provide additional product (0.41 g, total yield 3.41 g, 56%): MS (DCI/NH3) m/z 353 (M+H)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07872017B2 |
|---|
| 出典データセット | uspto-grants-2011_01 |
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| ORD ID | ord-14be6efbf7eb448b9aad427d153e60f1 |
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| 出典メモ | uspto-grants-2011_01 |
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