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Triethylamine → 5-Chloro-1-(phenoxymethyl)pyrimidin-2(1H)-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | (Chloromethoxy)benzene | HCID 81201 | — |
| 反応物 | 5-Chloro-2(1H)-pyrimidinone | HCID 108578 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 5-Chloro-1-(phenoxymethyl)pyrimidin-2(1H)-one | HCID 13062934 | — |
反応手順
5-Chloropyrimidin-2-one (5 mmol) and triethylamine (5 mmol) were stirred together in dichloromethane (50 ml). When all the solid had dissolved a solution of chloromethoxybenzene (see Preparation 2) (5 mmol) in dichloromethane (25 ml) was added with stirring at room temperature. The resultant mixture was stirred for 24 h at this temperature before the solvent was distilled off. The residue was triturated with water (30 ml), extracted into chloroform (3×20 ml), and the dried (MgSO4) solution evaporated to yield a mixture of the title compound and the O-alkylated isomer in the ratio 3:1; yield 7.00 g (85%). The N-isomer was separated by column chromatography on silica gel; m.p. 146° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04705791 |
| 出典データセット | uspto-grants-1987_11 |
| ORD ID | ord-4ac491f287534f00a08017e4a638c2b1 |
| 出典メモ | uspto-grants-1987_11 |