HRID471209

反应详情

EQUATION

反应方程式

HRID 471209 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of tert-butyl 4-(2-(2-chloroacetamido)ethyl)-4-hydroxypiperidine-1-carboxylate (example 89, step c) (0.3 g) in dry THF (18 mL) was added dropwise over 6 hours to a refluxing mixture of potassium tert-butoxide (1M in tert-butanol, 3 mL) and dry THF (60 mL). At the end of the addition the mixture was heated at reflux for a further 15 minutes and then cooled to room temperature. The mixture was partitioned between ethyl acetate and brine. The organic layer was dried over sodium sulphate, filtered and the solvent evaporated under reduced pressure. Tritruration with diethylether afforded the subtitled compound. Yield 0.117 g.

WORKUP

后处理

  1. additionAt the end of the addition the mixture
  2. temperaturewas heated
  3. temperatureat reflux for a further 15 minutes
  4. customThe mixture was partitioned between ethyl acetate and brine
  5. dry with materialThe organic layer was dried over sodium sulphate
  6. filtrationfiltered
  7. customthe solvent evaporated under reduced pressure