HRID988659

反应详情

EQUATION

反应方程式

HRID 988659 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of methyl 2-(1,4-dioxa-8-azaspiro[4.5]decan-8-ylcarbonyl)aminobenzoate (2.00 g, 6.25 mmol) in dioxane (30 mL) was treated with 5 N NaOH (12.5 mL). After 1 h, the mixture was poured into EtOAc and water, and the aqueous layer was washed with EtOAc. The pH of the aqueous layer was then adjusted to 2-3 by addition of 5 N HCl and washed with EtOAc (3×). The combined organic layers were washed with brine, dried with sodium sulfate, and concentrated, yielding the title compound; which was used without further purification.

WORKUP

后处理

  1. washthe aqueous layer was washed with EtOAc
  2. additionThe pH of the aqueous layer was then adjusted to 2-3 by addition of 5 N HCl
  3. washwashed with EtOAc (3×)
  4. washThe combined organic layers were washed with brine
  5. dry with materialdried with sodium sulfate
  6. concentrationconcentrated