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Triethylamine → N-(3-cyclopentyloxy-4-methoxyphenyl)-2,6-dichlorobenzamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 2,6-Dichlorobenzoyl chloride | HCID 78392 | — |
| 反応物 | 3-(Cyclopentyloxy)-4-methoxyaniline | HCID 2779334 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | N-(3-cyclopentyloxy-4-methoxyphenyl)-2,6-dichlorobenzamide | HCID 21187908 | 32.7% |
反応手順
A stirred solution of 3-cyclopentyloxy-4-methoxyaniline (1 g) and triethylamine (0.69 mL) in dry dichloromethane (20 mL) at 0° C. is treated dropwise with 2,6-dichlorobenzoyl chloride (1.17 g). After stirring at this temperature for 30 minutes, the mixture is warmed to room temperature and stirred for a further 3 hours. The organic layer is washed with water (100 mL), dried and concentrated. The residue is recrystallized from a mixture of isopropanol and hexane, to give N-(3-cyclopentyloxy-4-methoxyphenyl)-2,6-dichlorobenzamide (0.6 g), m.p. 184°-185° C. [Elemental analysis: C,60.2,H,5.0; N,3.6; Cl18.9%; calculated: C,60.0; H,5.0; N,3.7; Cl18.65%].
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05840724 |
| 出典データセット | uspto-grants-1998_11 |
| ORD ID | ord-2e58363523284db9afa04a2261945613 |
| 出典メモ | uspto-grants-1998_11 |