HRID2374445

反应详情

EQUATION

反应方程式

HRID 2374445 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a suspension of 3,4-dihydro-1H-isoquinoline-2,6-dicarboxylic acid 2-tert-butyl ester (96 mg, 0.348 mmol) in toluene (4 mL) is added SOCl2 (254 μL, 10 eq.). The mixture is heated to reflux for 3 hours. All the solvent is removed under reduced pressure. The residue is redissolved in toluene and evaporated to dryness twice to remove excess HCl and is dried under high vacuum for 2 hours to give crude 6-chlorocarbonyl-3,4-dihydro-1H-isoquinoline-2-carboxylic acid tert-butyl ester.

WORKUP

后处理

  1. temperatureThe mixture is heated
  2. temperatureto reflux for 3 hours
  3. customAll the solvent is removed under reduced pressure
  4. dissolutionThe residue is redissolved in toluene
  5. customevaporated to dryness twice
  6. customto remove excess HCl
  7. customis dried under high vacuum for 2 hours