関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 3-Phenyl-6-pyridazone | HCID 75106 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | (4-(2-Bromoethyl)phenoxy)(tert-butyl)dimethylsilane | HCID 636962 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-(4-(tert-Butyldimethylsilyloxy)phenethyl)-6-phenylpyridazin-3(2H)-one | HCID 59843023 | — |
反応手順
A mixture of (4-(2-bromoethyl)phenoxy)(tert-butyl)dimethylsilane (142 mg, 450 μmol), 6-phenyl-3(2h)-pyridazinone (116 mg, 676 μmol), and potassium carbonate (187 mg, 1351 μmol) in DMF (1.5 mL) was stirred at 40° C. for 18 h. The mixture was partioned between CH2Cl2 (20 mL) and 5% NaHCO3 (10 mL). The organic layer was dried with satd. NH4Cl and over MgSO4, and dried to a film from toluene under reduced pressure. The residue was purified on 40 g silica eluting with 0>2.5% MeOH/CH2Cl2. MS (ESI pos. ion) m/z (MH+): 407 (MH+). Calc'd exact mass for C24H30N2O2Si: 406.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08314087B2 |
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| 出典データセット | uspto-grants-2012_11 |
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| ORD ID | ord-879650c5aa864436b8a4494a15ce2108 |
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| 出典メモ | uspto-grants-2012_11 |
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