Diethyl Ether → HCID 73667394, compound

A mixture of potassium tert-butoxide (11.5 gm, 0.1 m), ether (400 ml), tert-butanol (15 ml) and absolute ethanol (15 ml) was refluxed for 1/2 hour to insure complete solution of the potassium tert-butoxide. To the hot solution was added 7-methoxy-1-tetralone (17.6 gms, 0.1 m) and the reaction mixture turned from yellow to dark brown. To this refluxing solution was added isopentyl nitrite (19 ml). During this addition external heating was not necessary because of the exothermic nature of the reaction. The reaction mixture was refluxed for 1/2 hour during which time the walls of the flask became coated with a brown solid. After cooling in an ice-bath, the solvent was removed by decantation. To the solid was added aqueous hydrogen chloride (1 N, 200 ml). After stirring 1/2 hour, the brown solid was filtered to yield 10 gms (50%) of product.

1. temperaturewas refluxed for 1/2 hour
2. additionDuring this addition
3. temperatureexternal heating
4. customwas not necessary because of the exothermic nature of the reaction
5. temperatureThe reaction mixture was refluxed for 1/2 hour during which time the walls of the flask
6. temperatureAfter cooling in an ice-bath
7. customthe solvent was removed by decantation
8. additionTo the solid was added aqueous hydrogen chloride (1 N, 200 ml)
9. filtrationthe brown solid was filtered

ORD record

ord-0f22921d68ab48c48f59c0bab6d037fc

Source dataset

uspto-grants-1983_12

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04420480