Organic Syntheses, CV 4, 350
Submitted by J. Colonge and R. Marey
1.
Checked by V. Boekelheide and H. Kaempfen.
1. Procedure
In a
100-ml., three-necked, round-bottomed flask, fitted with a sealed
mechanical stirrer, a
reflux condenser, and a
thermometer reaching to the bottom of the flask, are placed
37.6 g. (0.2 mole) of 2-methyl-2,5-decanediol (p.601) and
17 g. of 85% phosphoric acid. The limpid liquid obtained is heated and maintained at 125° for 40 minutes. Then the acidic lower layer is discarded, and the organic layer is washed with three or four 50-ml. portions of lukewarm distilled water.
Distillation of the resulting crude oil using a simple
fractionating column gives
32–33 g. (
94–97%) of pure
5,5-dimethyl-2-n-pentyltetrahydrofuran as a colorless liquid boiling at
31–33°/1.5 mm.;
nD25 1.4257 (Note
1).
2. Notes
3. Discussion
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