HRID2081242

反应详情

EQUATION

反应方程式

HRID 2081242 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1.9 g of 3-acetyl quinuclidine hydrochloride and 0.98 g of O-ethylhydroxylamine hydrochloride are heated for 20 minutes to reflux in 30 cm3 of methanol, followed by concentrating to dryness and purifying by chromatography on alumina (eluant: methylene chloride-methanol 9-1). The reaction medium is acidified using gaseous hydrochloric acid, then evaporated to dryness. After crystallizing from ethanol, filtering, and rinsing with ether, 1.3 g of expected product is recovered. M.p.=198°-200° C.

WORKUP

后处理

  1. concentrationby concentrating to dryness
  2. custompurifying by chromatography on alumina (eluant: methylene chloride-methanol 9-1)
  3. customevaporated to dryness
  4. customAfter crystallizing from ethanol
  5. filtrationfiltering
  6. washrinsing with ether, 1.3 g of expected product
  7. customis recovered