Entrya
Solvent
T (°C)
t (h)
Conversion of 1a (%) Yield of 3aa (%)
1 Toluene 100 5 2 n.d.
2 n-hexane 100 5 3 n.d.
3 CH2Cl2 100 5 13 n.d.
4 DMF 100 5 5 n.d.
5 MeCN 100 5 6 n.d.
6 THF 100 5 9 n.d.
7 none 100 5 100 93
8 none 80 24 13 7
9 none 120 5 100 81
10b none 100 5 97 73
11c none 100 5 100 81
12d none 100 5 100 90
13e none 100 5 100 91
aReaction conditions: 1a (0.3 mmol) and 2a (0.9 mmol) at 100 °C for 5 h under air. Corrected GC yields using n-dodecane as an internal standard were reported. n.d. = not detected. b1a/2a = 1:1. c1a/2a = 1:2. dUnder argon. eIn dark. aReaction conditions: 1a (0.3 mmol) and 2a (0.9 mmol) at 100 °C for 5 h under air. Corrected GC yields using n-dodecane as an internal standard were reported. n.d. = not detected. b1a/2a = 1:1. c1a/2a = 1:2. dUnder argon. eIn dark. aReaction conditions: 1a (0.3 mmol) and 2a (0.9 mmol) at 100 °C for 5 h under air. Corrected GC yields using n-dodecane as an internal standard were reported. n.d. = not detected. b1a/2a = 1:1. c1a/2a = 1:2. dUnder argon. eIn dark. aReaction conditions: 1a (0.3 mmol) and 2a (0.9 mmol) at 100 °C for 5 h under air. Corrected GC yields using n-dodecane as an internal standard were reported. n.d. = not detected. b1a/2a = 1:1. c1a/2a = 1:2. dUnder argon. eIn dark. aReaction conditions: 1a (0.3 mmol) and 2a (0.9 mmol) at 100 °C for 5 h under air. Corrected GC yields using n-dodecane as an internal standard were reported. n.d. = not detected. b1a/2a = 1:1. c1a/2a = 1:2. dUnder argon. eIn dark. aReaction conditions: 1a (0.3 mmol) and 2a (0.9 mmol) at 100 °C for 5 h under air. Corrected GC yields using n-dodecane as an internal standard were reported. n.d. = not detected. b1a/2a = 1:1. c1a/2a = 1:2. dUnder argon. eIn dark.