反应 #48208

反应方程式

Sodium hydride

4-([1,2,4]triazol-4-ylamino)-benzonitrile

ethyl acetate

2-benzyloxy-1-chloro-5-chloromethyl-3-methoxy-benzene

→

4-[(4-Benzyloxy-3-chloro-5-methoxy-benzyl)-[1,2,4]triazol-4-yl-amino]-benzonitrile

溶剂

DMF

water

反应条件

后处理

1. 1
   workup.ADDITIONwas added
2. 2
   其他The organic layer was separated
3. 3
   洗涤washed with water (2×50 mL) and brine (30 mL)
4. 4
   干燥The organic layer was dried over sodium sulphate
5. 5
   浓缩concentrated under reduced pressure
6. 6
   温度heated
7. 7
   温度to reflux for 5 minutes
8. 8
   过滤The white solid was filtered off
9. 9
   其他dried under high vacuum

实验过程

Sodium hydride (60%, 200 mg, 5.0 mmol) was added to a solution of 4-([1,2,4]triazol-4-ylamino)-benzonitrile (926 mg, 5.0 mmol) in DMF (20 mL) at r.t. The mixture was stirred for 1 h at this temperature and 2-benzyloxy-1-chloro-5-chloromethyl-3-methoxy-benzene (CAB02174, 1.49 g, 5.0 mmol) was added. The reaction mixture was stirred overnight and ethyl acetate (100 mL) and water (50 mL) were added. The organic layer was separated and washed with water (2×50 mL) and brine (30 mL). The organic layer was dried over sodium sulphate and concentrated under reduced pressure. The residue was suspended in 2-propanol (20 mL) and heated to reflux for 5 minutes. The white solid was filtered off after cooling to room temperature and dried under high vacuum. Yield: 1.76 g (79%).

来源