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Cyclopropylamine → 1-(4-Bromophenyl)-3-cyclopropylurea
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Cyclopropylamine | HCID 69828 | — |
| 反応物 | 4-Bromophenyl isocyanate | HCID 75609 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 1-(4-Bromophenyl)-3-cyclopropylurea | HCID 45860333 | — |
反応手順
Under a nitrogen atmosphere, tetrahydrofuran (80 ml) was added to 4-bromophenyl isocyanate 30 (10.0 g), and a solution of cyclopropylamine 1 (3.17 g) in tetrahydrofuran (20 ml) was added dropwise with stirring under ice-cooling. After the completion of the dropwise addition, the mixture was stirred at room temperature for 3 hrs, and the reaction mixture was concentrated under reduced pressure. Diethyl ether-hexane [1:1 (volume ratio), 100 ml] was added to the residue and, after stirring, the crystals were collected by filtration and dried to give 1-(4-bromo-phenyl)-3-cyclopropyl-urea 31 (12.9 ġ, over weight) as colorless crystals, which were used for the next step without purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08835443B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-44aea116db2f4ae2984a24fcb84ea4c0 |
| 出典メモ | uspto-grants-2014_09 |