HRID1373710

反应详情

EQUATION

反应方程式

HRID 1373710 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