HRID478947

反应详情

EQUATION

反应方程式

HRID 478947 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
2.5 °C

PROCEDURE

实验过程

To a cold (0-5° C.) suspension of Levodopa (197.2 g, 1.0 mol) in water (1.18 L) was added 32% aqueous HCl (159.5 g, 1.4 mol). The resulting solution was cooled to 0-5° C., and 37% formaldehyde water solution (243.24 g, 3.0 mol) was added. The resulting solution was allowed to warm to 20-25° C., and stirred at 20-25° C. for 10 h. The reaction solution was cooled to 0-5° C., and 2 N aqueous NaOH (700 mL, 1.4 mol) was slowly added to adjust pH to 5-5.5. White or light yellow solids precipitated during the addition. The resulting suspension was stirred at 0-5° C. for 2-3 h. The mixture was filtered, and rinsed with water (2×500 mL). The solids were dried under vacuum to give 199.52 g of a light yellow solid. Yield=95.3%.

WORKUP

后处理

  1. temperatureto warm to 20-25° C.
  2. temperatureThe reaction solution was cooled to 0-5° C.
  3. customWhite or light yellow solids precipitated during the addition
  4. stirringThe resulting suspension was stirred at 0-5° C. for 2-3 h
  5. filtrationThe mixture was filtered
  6. washrinsed with water (2×500 mL)
  7. customThe solids were dried under vacuum