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Acetonitrile → HCID 86680289、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetonitrile | HCID 6342 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Ethyl 6-(chloromethyl)pyridine-2-carboxylate | HCID 15614003 | — |
| 反応物 | (R)-3-benzhydryloxypyrrolidine | HCID 70647884 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | HCID 86680289 | HCID 86680289 | 54% |
反応手順
A mixture of 8.144 g of (R)-3-benzhydryloxypyrrolidine synthesized in Production Example 168, 7.701 g of a known compound ethyl 6-chloromethylpyridine-2-carboxylate, 69 mL of acetonitrile, and 9.0 mL of triethylamine was heated under reflux for 3 hours. After being allowed to cool down, the mixture was diluted with ethyl acetate. The diluted mixture was poured into a saturated saline solution, and the organic layer was collected by separation. The organic layer was washed with a saturated saline solution and dried over magnesium sulfate. The solvent was distilled off, and then the residue was purified by silica gel column chromatography (chloroform/acetone (volume ratio)=15:1 to 10:1) to give the title compound (7.22 g (54%)).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09365553B2 |
| 出典データセット | uspto-grants-2016_06 |
| ORD ID | ord-87ead9f29d3c44d09a18ab4650c96571 |
| 出典メモ | uspto-grants-2016_06 |