反応 #323122

反応方程式

3,4-dimethoxyphenylacetone

sodium cyanoborohydride

HCl

→

( VIII )

収率 96.5%

3-(3,4-Dimethoxyphenyl)-2-propylamine

収率 96.5%

溶媒

methanol

反応条件

後処理

1. 1
   その他the solvent is evaporated under reduced pressure
2. 2
   workup.DISSOLUTIONThe residue is dissolved in H2O (250 ml)
3. 3
   抽出the aqueous layer is extracted with ether (3×)
4. 4
   抽出extracted with CH2Cl2 (3×)
5. 5
   その他After drying
6. 6
   その他the solvent is evaporated under reduced pressure
7. 7
   workup.DISTILLATIONthe product is distilled at 112°-5°/0.5 mm

実験手順

A mixture of 3,4-dimethoxyphenylacetone (51.1 g, 0.26 m) is dissolved in methanol (780 ml), sodium cyanoborohydride (11.3 g, 0.18 m) is added and the mixture is stirred at room temperature for 67 hours. The reaction mixture is adjusted to pH 2 with concentrated HCl and the solvent is evaporated under reduced pressure. The residue is dissolved in H2O (250 ml), the aqueous layer is extracted with ether (3×) and then rendered alkaline with KOH and extracted with CH2Cl2 (3×). After drying, the solvent is evaporated under reduced pressure and the product is distilled at 112°-5°/0.5 mm to yield (VIII) (33.88 g, 67%).

出典