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. Author manuscript; available in PMC: 2012 Aug 24.
Published in final edited form as: Tetrahedron Lett. 2011 Aug 24;52(34):4375–4377. doi: 10.1016/j.tetlet.2011.05.114

Table 1.

Screening of solvents, reaction time and temperature for the synthesis of 7b

Base Conditiona Temp
(°C)
Time
(mins)
Yield b
(%)
- No solvent 90 15 Trace
- Ethanol 90 15 Trace
Piper
idene
Ethanol 90 15 80
TMP Ethanol 90 15 96
TMP No solvent 90 15 Trace
DBU
/
pyrid
ine
Ethanol 90 20 20
TMP Acetonitrile 90 15 76
TMP Acetonitrile 130 15 15
DBU Acetonitrile 90 30 Trace
TMP DMF 90 15 45
DMF 90 30 10
NMP
DBU DMF 120-
140
15 Trace
TMP Water 90 15 Trace
TMP Water 130 15 Trace
- Water 130 30 Trace
TMP Toluene 90 15 Trace
TMP Isopropanol 90 15 45
TMP THF 90 15 38
TMP n-Butanol 90 15 33
a

All the reaction was carried out in equimolar amount of each compound in 2 ml of solvent at 150 psi pressure.

b

Isolated yield