Isopropanol → Isopropyl cyanoacetate
反応式
[C:1]([CH2:3][C:4]([OH:6])=[O:5])#[N:2].[CH:7](O)([CH3:9])[CH3:8].CS(O)(=O)=O>>[C:1]([CH2:3][C:4]([O:6][CH:7]([CH3:9])[CH3:8])=[O:5])#[N:2]参加物
4
反応条件
- 温度
- 105 °C
実験手順
Cyanoacetic acid (85.5 g; 1.0 mol), isopropanol (80 g; 1.33 mol) and methanesulfonic acid (1.00 g; 0.01 mol) were introduced into a 500 ml flask. The mixture was slowly heated to a maximum of 105° C. while collecting distillates at 77-80° C. Additional isopropanol (220 g; 3.67 mol) was added to maintain the flask at 105-110° C. and the collection of distillates was continued at 77-80° C. After distilling off the unreacted isopropanol, the isopropyl cyanoacetate (bp 100° C./20 mm Hg) was collected as a clear liquid. The yield was 120 g (94.5% of theoretical and its purity was >99% (GC assay).
後処理
- distillationwhile collecting distillates at 77-80° C
- temperatureto maintain the flask at 105-110° C.
- distillationthe collection of distillates
- customwas continued at 77-80° C
- distillationAfter distilling off the unreacted isopropanol
- customthe isopropyl cyanoacetate (bp 100° C./20 mm Hg) was collected as a clear liquid
出典と根拠
- ORDレコード
- ord-484ce8834f104cb98a6fcd769f2d2602
- 出典データセット
- uspto-grants-2001_08
- 特許番号
- US06271410B1
反応ノート
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