HRID729610

反应详情

EQUATION

反应方程式

HRID 729610 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
22 °C

PROCEDURE

实验过程

To a cold solution of 4-(4-nitro-isoquinoline-1-yloxy)-piperidine-1-carboxylic acid tert-butyl ester (9.68 g, 25.9 mmol, 0° C.) in DCM (100 mL) add TFA (80 mL). Stir at 22° C. for 2 hours, then remove solvent under reduced pressure. Dissolve residue in DCM and treat with 1 N sodium hydroxide to pH˜14. Isolate the aqueous phase and extract twice with DCM. Combine the organic phases and dry with anhydrous sodium sulfate. Removal of the solvent gives (4-nitro-isoquinoline-1-yloxy)-piperidine (7.06 g, 99% yield, ES+ (m/z) 274.3 [M+H]).

WORKUP

后处理

  1. customIsolate the aqueous phase
  2. extractionextract twice with DCM
  3. dry with materialdry with anhydrous sodium sulfate
  4. customRemoval of the solvent