関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | HCID 178436445 | HCID 178436445 | — |
| 反応物 | HCID 178506895 | HCID 178506895 | — |
| 溶媒 | Pentane | HCID 8003 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | HCID 178436242 | HCID 178436242 | — |
反応手順
To a solution of 0.8 g (3.1 mmol) (E)-[1-(2-ethyl-6-methoxy-phenyl)-methylidene]-(1-isopropyl-2-methyl-propyl)-amine (Example 3 a)) in 3 ml dry THF cooled to −20° C. were added 9.62 ml of a 0.7M solution of isopropyl lithium in pentane drop-wise to keep temperature below 0° C. Then the mixture was stirred at −20° C. for further 30 min and the reaction quenched by addition of water. The aqueous phase was extracted with ethyl acetate, the combined extracts washed with brine, dried over Na2SO4, filtered and evaporated. Purification of the crude product by flash chromatography on silica gel with heptane as eluent provided 0.220 g (E)-[1-(2-ethyl-6-isopropyl-phenyl)-methylidene]-(1-isopropyl-2-methyl-propyl)-amine as colourless liquid: MS (ISP): 274.1 (M+H+.).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07875645B2 |
|---|
| 出典データセット | uspto-grants-2011_01 |
|---|
| ORD ID | ord-ed9b73ce17e54dcf999f7d6a2162a513 |
|---|
| 出典メモ | uspto-grants-2011_01 |
|---|