HRID621717

反应详情

EQUATION

反应方程式

HRID 621717 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3.7 g of the crude 2-methoxyacetyl-4-methylcyclohexanone, 1.68 g of cyanoacetamide and 1 ml of piperidine were mixed with 50 ml of ethanol and the obtained reaction mixture was heated under reflux for four hours. The crystals thus formed were filtered and purified to give 1.5 g of 4-cyano-2,3,5,6,7,8-hexahydro-1-methoxymethyl-7-methyl-3-oxoisoquinoline. m.p.: 205°-208° C. NMRδTMSDMSO-d6 :1.01 (3H, d), 1.2-2.0 (4H, m), 2.5-2.6 (1H, m), 2.7-2.9 (2H, m), 3.28 (3H, s), 4.32 (2H, s) and 11.86 (1H, s).

WORKUP

后处理

  1. customthe obtained reaction mixture
  2. temperaturewas heated
  3. temperatureunder reflux for four hours
  4. customThe crystals thus formed
  5. filtrationwere filtered
  6. custompurified