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Potassium Carbonate → 4'-Ethynyl-2-(trifluoromethyl)biphenyl
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2'-TrifluoroMethyl-Biphenyl-4-Carbaldehyde | HCID 1392653 | — |
| 反応物 | (1E)-1-diazo-1-dimethoxyphosphorylpropan-2-one | HCID 136023029 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 4'-Ethynyl-2-(trifluoromethyl)biphenyl | HCID 86661806 | 85.4% |
反応手順
To a stirred suspension of the product of Example 36, Step A, (0.21 g, 1 mmol) and K2CO3 (0.166 g, 1.1 mmol) in anhydrous MeOH (5 mL) was added a solution of dimethyl 1-diazo-2-oxopropylphosphonate (0.212 g, 1.1 mmol) in anhydrous MeOH (1 ml) and the mixture was stirred overnight at room temperature. The solvent was evaporated to dryness and the residue was diluted to 50 ml with EtOAc and washed with H2O. The organic layer was separated, dried over MgSO4, and filtered. The filtrate was passed through silica gel bead. The filtrate was evaporated to dryness to give the product (0.21 g, 85.4%), as creamy paste, which was used as such in next step. 1H-NMR (CDCl3) 3.11 (s, 1H); 7.25-7.31 (m, 3H); 7.44-7.55 (m, 4H); 7.73 (d, 1H, J=7.69 Hz).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09181182B2 |
| 出典データセット | uspto-grants-2015_11 |
| ORD ID | ord-bd7229f3ebbe4683b508cd737f42bc88 |
| 出典メモ | uspto-grants-2015_11 |