Pyridine → Trimethylsilyl crotonate
反応式
N1C=CC=CC=1.[C:7]([OH:12])(=[O:11])/[CH:8]=[CH:9]/[CH3:10].Cl[Si:14]([CH3:17])([CH3:16])[CH3:15]>CCOCC>[CH3:15][Si:14]([O:11][C:7](=[O:12])/[CH:8]=[CH:9]/[CH3:10])([CH3:17])[CH3:16]参加物
5
実験手順
Pyridine (138 g, 1.74 mol) is added dropwise to a stirred solution of crotonic acid (125 g, 1.45 mol), and chlorotrimethylsilane (189 g 1.74 mol) in ether (1.5 l) at room temperature. The reaction mixture is allowed to stir at room temperature overnight and the precipitate is removed by filtration. The filtrate is concentrated and the residue is distilled under reduced pressure. The product fraction is collected at 58–70° C. (25 mmHg) to give 180 g of the title compound (79%). GC-MS purity is 93.4%, 1HNMR is consistent with the structure.
後処理
- customthe precipitate is removed by filtration
- concentrationThe filtrate is concentrated
- distillationthe residue is distilled under reduced pressure
- customThe product fraction is collected at 58–70° C. (25 mmHg)
出典と根拠
- ORDレコード
- ord-0a1609a66b9f4e61b41fe5763184c4d9
- 出典データセット
- uspto-grants-2006_10
- 特許番号
- US07126025B2
反応ノート
読み込み中…