HRID1376898

反应详情

EQUATION

反应方程式

HRID 1376898 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of 6-hydroxy-3-oxo-2,3-dihydrobenzofuran of Example 10(a) (32 kg, 213 moles) in DMF (192 L) was added potassium carbonate (31.0 kg, 224 moles). After stirring for 5 min. at room temperature, benzyl bromide (45.2 kg, 264 moles) was added and the resulting mixture was stirred for 2 hours at room temperature. The mixture was poured into water (651 L), stirred for 30 minutes and the product collected by centrifugation. The crude solid was washed with water (580 L), 80% ethanol (100 L) and dried under vacuum to afford the desired product (49.1 kg, 95%) which was used without any further purification.

WORKUP

后处理

  1. stirringthe resulting mixture was stirred for 2 hours at room temperature
  2. stirringstirred for 30 minutes
  3. customthe product collected by centrifugation
  4. washThe crude solid was washed with water (580 L), 80% ethanol (100 L)
  5. customdried under vacuum