Hydrochloric Acid → Dimethyl(1-octenyl)(2-pyridyl)silane

温度

40 °C

To 1.0 ml of diethyl ether were added 10 mg (0.25 μmol) of bis(cyclooctadiene)platinum, 13 mg (0.50 μmol) of triphenylphosphine and 165 mg (1.5 mmol) of 1-octyne, and 69 mg (0.5 mmol) of dimethyl(2-pyridyl)silane was added dropwise thereto at room temperature over 1 hour. Further, the mixture was continued to be stirred for 6 hours at an inner temperature of 40° C., followed by the addition of 6 ml of 1N hydrochloric acid and 5 ml of diethyl ether. After the mixture was stirred for 30 minutes, it was left stand and separated into the organic and aqueous layers. The organic layer was extracted with five portions of 6 ml of 1N hydrochloric acid, and the resulting aqueous layers were combined together and turned basic with the addition of sodium hydroxide pellets. This aqueous layer was extracted with three portions of 10 ml of diethyl ether. The resulting organic layer was dried over magnesium sulfate and the solvent was evaporated off under reduced pressure to give 112 mg of dimethyl(1-octenyl)(2-pyridyl)silane. Yield: 90%.

1. additionwas added dropwise
2. stirringAfter the mixture was stirred for 30 minutes
3. waitit was left stand
4. customseparated into the organic and aqueous layers
5. extractionThe organic layer was extracted with five portions of 6 ml of 1N hydrochloric acid
6. additionturned basic with the addition of sodium hydroxide pellets
7. extractionThis aqueous layer was extracted with three portions of 10 ml of diethyl ether
8. dry with materialThe resulting organic layer was dried over magnesium sulfate
9. customthe solvent was evaporated off under reduced pressure

ORDレコード

ord-ec285a85be014e9ebe6187b6299f4e8d

出典データセット

uspto-grants-2003_04

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US06548673B1