関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 1-Chloro-4-[(chloromethoxy)methyl]benzene | HCID 12946592 | — |
| 反応物 | 5-(Trifluoromethyl)pyrimidin-2(1H)-one | HCID 13317027 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1-(4-Chlorobenzyloxy)methyl-5-trifluoromethylpyrimidin-2-one | HCID 13317032 | 91% |
反応手順
Triethylamine (1 mmol) was added to a mixture of 5-trifluoromethyl pyrimidin-2-one (see Preparation 11 of European Patent Publication Ser. No. 0 056 319) (1 mmol) in dichloromethane (10 ml) and the solution stirred for 5 minutes before 4-chlorobenzyl chloromethyl ether (see Preparation 5a and 5b) (1 mmol) in dichloromethane (2 ml) was added. The mixture was stirred at room temperature overnight and at 40° C. for 3 hours before the solvent was distilled off and the residue triturated with water. The product was extracted into chloroform, dried (MgSO4) and evaporated. The residue was washed with ether and dried; yield 91%, m.p. 120° C. 1H NMR (CDCl3): δ4.64 (CH2Ph), 5.38 (NCH2), 7.24 (Ph), 8.11 (H-4, J 3 Hz), 8.74 (H-6, J 3 Hz). IR (KBr): 1680 cm-1 (CO).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04539324 |
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| 出典データセット | uspto-grants-1985_09 |
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| ORD ID | ord-ed057300f21141de91e5e4b67fea634b |
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| 出典メモ | uspto-grants-1985_09 |
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