反応 #58717

反応方程式

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

収率 9.0%

溶媒

methanol

NaHCO3

反応条件

後処理

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

実験手順

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.

出典