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Water → 1-(3-Bromophenyl)-3-heptyl-1-methylurea
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | n-Heptyl isocyanate | HCID 138341 | — |
| 反応物 | Benzenemethanamine, 3-bromo- | HCID 457587 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 1-(3-Bromophenyl)-3-heptyl-1-methylurea | HCID 11616837 | 77% |
反応手順
3.2 mL (20 mmol) of heptyl isocyanate are added to a solution of 2.5 g (13 mmol) of (3-bromophenyl)methylamine (prepared according to Example 24f) in 10 mL of tetrahydrofuran in the presence of 2 mL of triethylamine. The reaction mixture is stirred for 12 hours at room temperature. The reaction is stopped by addition of 2 mL of water and extraction with ethyl acetate. The organic phases are combined and dried over sodium sulfate. The solvents are evaporated off and the residue is then purified by chromatography on a column of silica eluted with a 70/30 heptane/ethyl acetate mixture. 3.4 g (77%) of 1-(3-bromophenyl)-3-heptyl-1-methylurea are obtained in the form of a solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08383652B2 |
| 出典データセット | uspto-grants-2013_02 |
| ORD ID | ord-1fe78045841c41bd8e93be2ba27e033d |
| 出典メモ | uspto-grants-2013_02 |