化工社化工社 化学情報印刷レポート · 研究参考用
Triethylamine → tert-Butyl (2E)-3-{4-[(4-hydroxyphenyl)(tetrahydro-4H-pyran-4-ylidene)methyl]phenyl}-2-methylprop-2-enoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | tert-Butyl methacrylate | HCID 11448 | — |
| 反応物 | Tri-o-tolylphosphine | HCID 80271 | — |
| 反応物 | 4-[(4-Bromophenyl)(tetrahydro-4H-pyran-4-ylidene)methyl]phenol | HCID 68654197 | — |
| 反応物 | tert-Butyl (2E)-3-{4-[(4-hydroxyphenyl)(tetrahydro-4H-pyran-4-ylidene)methyl]phenyl}prop-2-enoate | HCID 86613505 | — |
| 触媒 | palladium(II) acetate | HCID 167845 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | tert-Butyl (2E)-3-{4-[(4-hydroxyphenyl)(tetrahydro-4H-pyran-4-ylidene)methyl]phenyl}-2-methylprop-2-enoate | HCID 86613507 | 59% |
反応手順
Following the procedure described for compound 47, from 4-[(4-bromophenyl)(tetrahydro-4H-pyran-4-ylidene)methyl]phenol (46) (0.101 g, 0.293 mmole), tert-butyl methacrylate (0.095 mL, 0.585 mmole), P(o-tolyl)3 (0.0092 g, 0.0302 mmole), Et3N (0.125 mL, 0.897 mmole), Pd(OAc)2 (0.0038 g, 0.0169 mmole) and DMF (1.5 mL) yielded compound 59 (0.070 g, 59%) as a white solid. 1H NMR (CDCl3): δ 7.55 (s, 1H), 7.31 (d, J=8.1 Hz, 2H), 7.11 (d, J=8.1 Hz, 2H), 6.98 (d, J=8.5 Hz, 2H), 6.76 (d, J=8.5 Hz, 2H), 4.91 (s, 1H), 3.73 (m, 4H), 2.41 (m, 4H), 1.58 (s, 3H), 1.54 (s, 9H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07560589B2 |
| 出典データセット | uspto-grants-2009_07 |
| ORD ID | ord-d0a95525806e408d8c8cdd5f5aaa91a3 |
| 出典メモ | uspto-grants-2009_07 |