化工社化工社 化学情報印刷レポート · 研究参考用
Sodium Carbonate → (4-(2-Chloroethoxy)phenyl)(3-fluoro-4-hydroxyphenyl)methanone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | (4-(2-Chloroethoxy)phenyl)(3-fluoro-4-methoxyphenyl)methanone | HCID 89656203 | — |
| 溶媒 | Hydrogen Bromide | HCID 260 | — |
| 生成物 | (4-(2-Chloroethoxy)phenyl)(3-fluoro-4-hydroxyphenyl)methanone | HCID 89656051 | 51% |
反応手順
(4-(2-Chloroethoxy)phenyl)(3-fluoro-4-methoxyphenyl)methanone from the previous step in 20 mL 40% HBr was refluxed for 1 h., neutralized with solid Na2CO3 at 0° C., and extracted with EtOAc. The extract was washed with brine, dried, concentrated, and purified by column chromatography (eluent: petroleum ether/EtOAc=5/1 to 2/1) over silica gel to give the subtitle compound (731 mg, 51% yield for 3 steps) as a yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09309211B2 |
| 出典データセット | uspto-grants-2016_04 |
| ORD ID | ord-199cf749595d45de957133c948a279da |
| 出典メモ | uspto-grants-2016_04 |