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Potassium Phosphate, Tribasic → [4-(3-Chloropyrazin-2-yl)phenyl]acetic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Phosphate, Tribasic | HCID 62657 | — |
| 反応物 | Tricyclohexylphosphine | HCID 75806 | — |
| 反応物 | 2,3-Dichloropyrazine | HCID 78575 | — |
| 反応物 | 2-(4-(4,4,5,5-Tetramethyl-1,3,2-dioxaborolan-2-yl)phenyl)acetic Acid | HCID 3719002 | — |
| 触媒 | Bis(dibenzylideneacetone)palladium | HCID 9811564 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | [4-(3-Chloropyrazin-2-yl)phenyl]acetic acid | HCID 59535937 | — |
反応手順
To a solution of 0.10 g (0.38 mmol) [4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)phenyl]acetic acid in 1.2 ml of dioxane was added 0.17 g (1.15 mmol) of 2,3-dichloropyrazine, 2.57 mg (0.009 mmol) of tricyclohexylphosphine, 3.5 mg (0.004 mmol) of Pd2(dba)3, and 0.51 ml (1.27 M, 0.65 mmol) of aqueous potassium phosphate solution. The resulting suspension was degassed for 10 minutes. After 30 min in the microwave at 100° C., the reaction mixture was cooled, acidified with 1N HCl, extracted with ethyl acetate, and washed with brine. The organic layer was dried over Na2SO4, filtered and concentrated in vacuo to afford crude [4-(3-chloropyrazin-2-yl)phenyl]acetic acid. ES-MS M+1=249.1.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08637513B2 |
| 出典データセット | uspto-grants-2014_01 |
| ORD ID | ord-1df42e582d8249e392fc58df6c37ccc4 |
| 出典メモ | uspto-grants-2014_01 |