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Potassium Carbonate → 4-(3-Butyn-1-yl)benzenemethanol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 3-(4-(Hydroxymethyl)phenyl)propanal | HCID 53425276 | — |
| 反応物 | (1E)-1-diazo-1-dimethoxyphosphorylpropan-2-one | HCID 136023029 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 4-(3-Butyn-1-yl)benzenemethanol | HCID 23596609 | — |
反応手順
8.5 g (61.5 mmol) K2CO3 are added to a solution of 5.0 g (30.4 mmol) 3-(4-hydroxymethyl-phenyl)-propionaldehyde in 100 mL MeOH and then a solution of 7.0 g (36.4 mmol) dimethyl (1-diazo-2-oxo-propyl)-phosphonate in 50 mL MeOH is added dropwise and stirred for 3 h at RT. The reaction mixture is diluted with 200 mL EtOAc, washed with 80 mL saturated NaHCO3 solution, the aqueous phase extracted with 100 mL EtOAc and the combined organic phases are dried over Na2SO4. After the desiccant and solvent have been eliminated the residue is purified by chromatography on silica gel (cyc/EtOAc 3:1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08618132B2 |
| 出典データセット | uspto-grants-2013_12 |
| ORD ID | ord-c2b8312956604758a7c076246942cb16 |
| 出典メモ | uspto-grants-2013_12 |