HRID351403

反应详情

EQUATION

反应方程式

HRID 351403 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
35 °C

PROCEDURE

实验过程

2-Amino-5-chlorobenzamide (Avocado) (3.00 g, 17.5 mmol, 1.0 eq.) was suspended in 105 mL of H2O and 1.75 mL of HOAc at rt. A 12 mL solution of H20 and sodium cyanate (2.80 g, 43.0 mmol, 2.46 eq.) was then added slowly. Stirred at 35° C. for 1 hour. Added 31.26 mL of 1.0 N NaOH slowly. Solids precipitated. Cooled to 0C. Carefully added conc. HCl to pH=3. Filtered solids. Solids were then stirred in diethyl ether then refiltered and pumped under high vacuum to give 3.36 grams of tan solids as product. LCMS detects (M+H)+=197.

WORKUP

后处理

  1. customat rt
  2. customSolids precipitated
  3. temperatureCooled to 0C
  4. filtrationFiltered solids
  5. stirringSolids were then stirred in diethyl ether