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. 2021 Jan 31;36(1):549–560. doi: 10.1080/14756366.2020.1759582

Table 1.

The optimisation of conditions for the preparation of compound 9–8.

Inline graphic
Entry Heating Temp (∘C) Time (min) Yield (%)
1a Oil bath Reflux 60 Trace
2a Oil bath Reflux 360 10c
3a Oil bath Reflux 600 30c
4a Oil bath Reflux 720 41c
5a Oil bath Reflux 960 52d
6b MW 120 20 45c
7b MW 130 10 50d
8 b MW 130 20 67 d
9b MW 130 30 62d
10b MW 140 20 60d
a

Reaction conditions: ethyl 2-((3-bromophenyl)amino)-2-oxoacetate (1 mmol), Ph3P (1.5 mmol), CCl4 (5 ml).

b

Reaction conditions: ethyl 2-((3-bromophenyl)amino)-2-oxoacetate (1 mmol), Ph3P (1.5 mmol), CCl4 (5 ml), MW.

c

The yields were determined by HPLC.

d

Isolated yields.