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Water → N-[4-(4-Piperidinomethyl-2-pyridyloxy)-cis-2-butenyl]-2-chloroacetamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Chloroacetyl chloride | HCID 6577 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 2-Buten-1-amine, 4-[[4-(1-piperidinylmethyl)-2-pyridinyl]oxy]-, (Z)- | HCID 13672473 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | N-[4-(4-Piperidinomethyl-2-pyridyloxy)-cis-2-butenyl]-2-chloroacetamide | HCID 67725626 | 73% |
反応手順
0.54 ml of triethylamine was added to a solution of 1.00 g of 4-(4-piperidinomethyl-2-pyridyloxy)-cis-2-butenylamine in 20 ml of ethyl acetate, and the resulting mixture was cooled. 0.31 ml of 2-chloroacetyl chloride were then added to the mixture. The reaction mixture was then stirred at room temperature for 1 hour, after which it was mixed with water, and the aqueous mixture was extracted with ethyl acetate. The extract was concentrated by evaporation under reduced pressure, and the residue was purified by column chromatography through silica gel, using a 1:19 by volume mixture of methanol and ethyl acetate as the eluent, to give 0.94 g (yield 73%) of the title compound as an oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05616579 |
| 出典データセット | uspto-grants-1997_04 |
| ORD ID | ord-51964fb84fdc4a97a1a24b02c9b357e6 |
| 出典メモ | uspto-grants-1997_04 |