Trimethylsilyl cyanide → 7-Methoxy-4-cyano chrom-3-ene
反応式
[CH3:1][O:2][C:3]1[CH:12]=[C:11]2[C:6]([C:7](=O)[CH2:8][CH2:9][O:10]2)=[CH:5][CH:4]=1.C[Si]([C:18]#[N:19])(C)C>CC#N>[CH3:1][O:2][C:3]1[CH:12]=[C:11]2[C:6]([C:7]([C:18]#[N:19])=[CH:8][CH2:9][O:10]2)=[CH:5][CH:4]=1参加物
4
実験手順
7-Methoxy-4-chromanone (7 g) was added to trimethylsilyl cyanide (TMSCN) (7 ml), CH3CN (10 ml) and a catalytic amount of ZnIhd 2 and refluxed for 2 hrs. The reaction was cooled, evaporated to dryness, then isopropyl alcohol saturated with HCl(g) (100 ml) was added and this solution refluxed 2 hrs. The reaction was cooled, evaporated to dryness, and saturated aqueous NaCl added. This was then extracted with CH2Cl2, the organic layer separated, dried (Na2SO4), filtered and evaporated affording 7.1 g of product IR(CHCl3) 2218 cm-1 :
後処理
- temperaturea catalytic amount of ZnIhd 2 and refluxed for 2 hrs
- temperatureThe reaction was cooled
- customevaporated to dryness
- additionisopropyl alcohol saturated with HCl(g) (100 ml) was added
- temperaturethis solution refluxed 2 hrs
- temperatureThe reaction was cooled
- customevaporated to dryness, and saturated aqueous NaCl
- additionadded
- extractionThis was then extracted with CH2Cl2
- customthe organic layer separated
- dry with materialdried (Na2SO4)
- filtrationfiltered
- customevaporated
出典と根拠
- ORDレコード
- ord-92a786095dcd44c5a31c3878f1a2a926
- 出典データセット
- uspto-grants-1992_02
- 特許番号
- US05089519
反応ノート
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