- Synthetic Method of Hexahydro-2-(1H)-azocinone
-
Hexahydro-2-(1H)-azocinone(CAS no.: ), which is also known as 2(1H)-Azocinone, hexahydro-, could be produced through the following synthetic routes.
.gif)
A 100-mL, three-necked flask is equipped with a magnetic stirring bar, a pressure-equalizing dropping funnel, and a reflux condenser connected to a nitrogen flow line. The system is dried with a heat gun while it is flushed with dry nitrogen. The reaction vessel is then cooled in a water bath while a light positive pressure of nitrogen is maintained. The flask is charged with hydroxylamine-O-sulfonic acid (8.48 g, 0.075 mol) and 95–97% formic acid (45 mL). A solution of (5.61 g, 0.05 mol) in 15 mL of 95–97% formic acid is added with stirring over a 3-min period. After addition is complete, the reaction mixture is heated under reflux for 5 hr and then cooled to room temperature. The reaction mixture is quenched with 75 mL of ice–water. The aqueous solution is slowly neutralized to pH 7 with 6 N sodium hydroxide and extracted with three 100-mL portions of chloroform. The combined organic layers are dried with anhydrous magnesium sulfate. After removal of the solvent on a rotary evaporator, the product hexahydroazocinone is purified by distillation to give 4.6 g (72%), bp 94–96°C/0.2 mm, (short-path apparatus), lit bp 133–135°C/4 mm.
Prev:No record
Next:No record - 【Back】【Close 】【Print】【Add to favorite 】
-
Health and Chemical more >
-
Hot Products
- 10049-21-5 Sodium dihydrogen phosphate monohydrate
- 14464-46-1 SILICA
- 65141-46-0 Nicorandil
- 140-10-3 trans-Cinnamic acid
- 16096-30-3 PROPYLENE GLYCOL DIGLYCIDYL ETHER
- 3150-24-1 4-Nitrophenyl-beta-D-galactopyranoside
- 4415-87-6 Cyclobutane-1,2,3,4-tetracarboxylic dianhydride
- 101357-36-2 1,2,3,4-Butanetetracarboxylic acid, polymer with 2,2-bis(hydroxymethyl)-1,3-propanediol and 3-hydroxy-2,2-dimethylpropanal, 1,2,2,6,6-pentamethyl-4-piperidinyl ester
- 91-44-1 2H-1-Benzopyran-2-one,7-(diethylamino)-4-methyl-
- 1544-85-0 2,2-Difluoro-5-aminobenzodioxole
- 7786-30-3 Magnesium chloride
- 58857-49-1 Poly(oxy-1,2-ethanediyl), .alpha.-(9Z)-9-octadecenyl-.omega.-hydroxy-, phosphate, ammonium salt


