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Sodium Carbonate → 2-Chloro-4-(5-chloro-2-methoxyphenyl)benzoic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | 1,4-Dioxane | HCID 31275 | — |
| 反応物 | 5-Chloro-o-anisic acid | HCID 76970 | — |
| 反応物 | 4-Bromo-2-chlorobenzoic acid | HCID 108829 | — |
| 触媒 | Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+) | HCID 178418228 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 2-Chloro-4-(5-chloro-2-methoxyphenyl)benzoic acid | HCID 53227577 | 79.2% |
反応手順
4-bromo-2-chlorobenzoic acid (0.4 g), 5-chloro-2-methoxybenzoic acid (0.4 g), Pd(dppf)Cl2 (0.12 g), sodium carbonate (0.9 g), dioxan (15 ml) and methanol (5 ml) were charged to a flask and heated at reflux for 16 h. Cooled to room temp and filtered (hyflo). The filtrate was concentrated in vacuo, then dissolved in ethyl acetate. The suspension was made basic by addition of dilute NaOH. The aqueous layer was separated and acidified using 2M HCl, extracted with EtOAc, dried (MgSO4) and evaporated in vacuo to give the sub-title compound Yield 0.4 g
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07737135B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-ab2b160fe763407f91689f6ef0679c8c |
| 出典メモ | uspto-grants-2010_06 |