Triethylsilane → HCID 18545868、化合物
反応式
[CH3:1][C:2]1[C:7]2[CH:8]([C:12]([OH:14])=[O:13])[CH2:9][C:10](=O)[C:6]=2[CH:5]=[CH:4][CH:3]=1.C([SiH](CC)CC)C>FC(F)(F)C(O)=O>[CH3:1][C:2]1[CH:3]=[CH:4][CH:5]=[C:6]2[C:7]=1[CH:8]([C:12]([OH:14])=[O:13])[CH2:9][CH2:10]2参加物
4
実験手順
To a solution of 12a (100 g) in trifluoroacetic acid is added trietylsilane (141 g). The mixture was stirred for 72 hours at room temperature and was then evaporated in vacuo the residue was dissolved in ethyl acetate and was extracted with dilute NaOH solution. The aqueous phase was washed with etyl acetate and was then acidified with concentrated hydrochloric acid. Conventional work up with ethyl acetate gave 80.4 g of crude product. Purification on silica gel eluted with ethyl acetate-heptane-acetic acid gave the title compound (76.6 g).
後処理
- customwas then evaporated in vacuo the residue
- dissolutionwas dissolved in ethyl acetate
- extractionwas extracted with dilute NaOH solution
- washThe aqueous phase was washed with etyl acetate
- customgave 80.4 g of crude product
- customPurification on silica gel
- washeluted with ethyl acetate-heptane-acetic acid
出典と根拠
- ORDレコード
- ord-3086b06997da4e0799f585676bc84d58
- 出典データセット
- uspto-grants-2002_03
- 特許番号
- US06352988B2
反応ノート
読み込み中…