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1-Butanamine, N,N-dibutyl-, hydrochloride (1:1) → (2-Butyl-5-nitro-1-benzofuran-3-yl)(4-hydroxyphenyl)methanone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1-Butanamine, N,N-dibutyl-, hydrochloride (1:1) | HCID 80570 | — |
| 反応物 | (2-Butyl-5-nitrobenzofuran-3-yl)(4-methoxyphenyl)methanone | HCID 22595055 | — |
| 生成物 | (2-Butyl-5-nitro-1-benzofuran-3-yl)(4-hydroxyphenyl)methanone | HCID 11473234 | — |
反応手順
1.50 g (4.25 mmol) of 2-n-butyl-3-(4-methoxybenzoyl)-5-nitrobenzofuran (Ia) were dissolved in 4.71 g (21.2 mmol) of tri-n-butylamine-hydrochloride at 150° C. After 16 h LC-MS analysis indicated the complete consumption of the starting material and the reaction mixture was cooled to room temperature. After addition of 20 ml of water and 50 ml MTBE the phases were separated, the organic layer was washed once with 25 ml of 1M HCl and 20 ml of water, dried over MgSO4 and evaporated. Flash chromatography gave the title compound which crystallized to yield 1.10 g (76%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08658808B2 |
| 出典データセット | uspto-grants-2014_02 |
| ORD ID | ord-8f38abff3dc54b45b977ff1b4049ff33 |
| 出典メモ | uspto-grants-2014_02 |