関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Methoxyethylamine | HCID 8018 | — |
| 反応物 | Stilbene oxide | HCID 28649 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | beta-[(2-Methoxyethyl)amino]-alpha-phenylbenzeneethanol | HCID 411476 | 80% |
反応手順
A mixture of trans-stilbene oxide (3.93 g, 0.020 mole) and 2-methoxyethylamine (4.51 g, 0.060 mole) was heated at 125° C. for 2 hours with an oil bath. A mass spectra analysis showed no title compound was present. The mixture was heated for another 2 hours at 150° C. The mixture was poured into water (using methanol rinse) to obtain an off-white solid. NMR analysis showed the solid contained approximately 60% unreacted stilbene oxide. The mixture was added to another 4.51 g (0.060 mole) of 2-methoxy ethylamine and the mixture heated at 135° C. for 4 hours in a stainless-steel bomb. After cooling, the reaction mixture was shown by NMR analysis to contain 20% stilbene oxide and 80% of the title compound. The solid was recrystallized from toluene to give 2.92 g (54%) of a white solid, m.p. 137°-139° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US04803200 |
|---|
| 出典データセット | uspto-grants-1989_02 |
|---|
| ORD ID | ord-ddd1ff081f7947d5957272c46c029e9e |
|---|
| 出典メモ | uspto-grants-1989_02 |
|---|