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Boiling Point or [Melting Point], °C. |
Yield, % |
---|---|---|
5 |
34–37 (0.8 mm.) |
98 |
7 |
62 (0.4 mm.) |
83 |
8 |
a |
87 |
9 |
a |
73 |
10 |
[54–55] |
81 |
11 |
b |
79 |
12 |
[42–43] |
57 |
a Liquid, purified by crystallization from ether at −60°. |
||
b Liquid, purified by crystallization from ethanol at −20°. |
Appendix
Compounds Referenced (Chemical Abstracts Registry Number)
sodium salt of the hydroxymethylene
2-Diazocycloalkanones
sodium salt of an α-(hydroxymethylene) ketone
ethanol (64-17-5)
hydrochloric acid (7647-01-0)
Benzene (71-43-2)
methanol (67-56-1)
ether (60-29-7)
Cyclohexanone (108-94-1)
sodium sulfate (7757-82-6)
potassium hydroxide (1310-58-3)
diethylamine (109-89-7)
sodium azide (26628-22-8)
dichloromethane (75-09-2)
Tetrahydrofuran (109-99-9)
triethylamine (121-44-8)
2-(hydroxymethylene)cyclohexanone (823-45-0)
p-Toluenesulfonyl chloride (98-59-9)
2-Diazocyclohexanone, Cyclohexanone, 2-diazo- (3242-56-6)
p-toluenesulfonyl azide (941-55-9)