反应 #58717

反应方程式

3-(4′-acetyl-biphenyl-4-yl)-N-(4-chloro-phenyl) -acrylamidine

methoxylamine hydrochloride

sodium acetate

→

N-(4-chloro-phenyl)-3-[4′-(1-methoxyimino-ethyl)-biphenyl-4-yl]-acrylamidine

收率 9.0%

溶剂

methanol

NaHCO3

反应条件

后处理

1. 1
   温度was heated under microwave (100 W, 5 min)
2. 2
   萃取was extracted with two 10 mL portions of ethyl acetate
3. 3
   洗涤The combined organic extracts were washed with 10 mL of brine
4. 4
   干燥dried over Na2SO4
5. 5
   过滤filtered
6. 6
   浓缩concentrated
7. 7
   其他The residue was purified by preparative TLC
8. 8
   洗涤eluting with 70% ethyl acetate in hexanes plus 1% NH4OH

实验过程

A mixture of 0.04 g (0.11 mmol) of 3-(4′-acetyl-biphenyl-4-yl)-N-(4-chloro-phenyl) -acrylamidine, 0.028 g (0.33 mmol) of methoxylamine hydrochloride and 0.027 g (0.33 mmol) of sodium acetate in 3 mL of methanol was heated under microwave (100 W, 5 min). Diluted with 20 mL of NaHCO3, it was extracted with two 10 mL portions of ethyl acetate. The combined organic extracts were washed with 10 mL of brine, dried over Na2SO4, filtered and concentrated. The residue was purified by preparative TLC eluting with 70% ethyl acetate in hexanes plus 1% NH4OH to give 0.004 g of N-(4-chloro-phenyl)-3-[4′-(1-methoxyimino-ethyl)-biphenyl-4-yl]-acrylamidine.

来源