HRID621711

反应详情

EQUATION

反应方程式

HRID 621711 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1.02 g of 2-acetyl-4-methoxycyclohexanone and 0.462 g of cyanoacetamide were mixed with 5 ml of ethanol and a small amount of piperidine was added thereto. The obtained reaction mixture was heated under reflux for two hours. The crystals thus precipitated were filtered and recrystallized from methanol to give 0.42 g of 4-cyano-2,3,5,6,7,8-hexahydro-7-methoxy-1-methyl-3-oxoisoquinoline. m.p. 257°-259° C. NMRTMSCF3COOH : 2.25 (2H, m), 2.57 (3H, s), 2.97 (2H, m), 3.20 (2H, m), 3.66 (3H, s) and 4.16 (1H, m).

WORKUP

后处理

  1. customThe obtained reaction mixture
  2. temperaturewas heated
  3. temperatureunder reflux for two hours
  4. customThe crystals thus precipitated
  5. filtrationwere filtered
  6. customrecrystallized from methanol