HRID1292989

反应详情

EQUATION

反应方程式

HRID 1292989 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A stirred mixture of 1-(5-chloro-2-nitrophenyl)-4-methylpiperazine (1.0 mmol) and chloromethyl-(4-fluorophenyl)sulfone (1.0 mmol) in THF is treated with 2.2 mL of a 1M KOt-Bu (2.2 mmol) solution in THF at −78° C., warmed to room temperature over a 2 h period, quenched with acetic acid and concentrated in vacuo. The resultant residue is partitioned between EtOAc and aqueous Na2CO3. The phases are separated and the aqueous phase is extracted with EtOAc. The organic phase is combined with the extracts, dried over Na2SO4 and concentrated to dryness in vacuo to afford the title product.

WORKUP

后处理

  1. customquenched with acetic acid
  2. concentrationconcentrated in vacuo
  3. customThe resultant residue is partitioned between EtOAc and aqueous Na2CO3
  4. customThe phases are separated
  5. extractionthe aqueous phase is extracted with EtOAc
  6. dry with materialdried over Na2SO4
  7. concentrationconcentrated to dryness in vacuo