HRID1868627

反应详情

EQUATION

反应方程式

HRID 1868627 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Methyl N-((6-chloro-4-hydroxy-2-oxo-2′,3′,5′,6′-tetrahydro-2H-spiro[naphthalene-1,4′-pyran]-3-yl)carbonyl)glycinate (0.684 g, 1.79 mmol, 1.0 eq.) was suspended in water (10.0 mL) and treated with lithium hydroxide monohydrate (0.227 g, 5.40 mmol). After 30 minutes at ambient temperature, the resulting homogeneous mixture was quenched with 1N HCl solution to pH=2. The white solid that precipitated upon acidification was collected by vacuum filtration and washed with 1:1 H2O/acetone (2×2.0 mL). The product was dried under vacuum at 80° C. for 24 hours to give the title compound in quantitative yield. MS m/e=366.0 (M+H)+. Calculated for C17H16ClNO6 365.07.

WORKUP

后处理

  1. customthe resulting homogeneous mixture was quenched with 1N HCl solution to pH=2
  2. customThe white solid that precipitated upon acidification
  3. filtrationwas collected by vacuum filtration
  4. washwashed with 1:1 H2O/acetone (2×2.0 mL)
  5. customThe product was dried under vacuum at 80° C. for 24 hours