Diethylamine → Chlorobis(diethylamino)phosphine

In a 300 ml three-necked flask equipped with a dropping funnel and a magnetic stirrer, 10.0 g (0.0728 mol) of phosphorus trichloride and 100 ml of anhydrous diethyl ether were charged at room temperature in a nitrogen gas atmosphere, and the mixture was cooled to 5° C. or less in an ice bath. While the resulting reaction mixture was stirred, 30.0 ml (0.291 mol) of diethylamine were slowly added dropwise to the reaction mixture over 3 hours. The resulting crystals were filtered off under pressure in a nitrogen gas atmosphere. After the crystals were washed with anhydrous diethyl ether three times, they were purified by vacuum-distillation (0.4 kPa, 77.8-78.2° C.), and 8.07 g of chlorobis(diethylamino)phosphine were obtained in the form of a transparent liquid; the yield was 53%.

1. customIn a 300 ml three-necked flask equipped with a dropping funnel and a magnetic stirrer
2. temperaturethe mixture was cooled to 5° C. or less in an ice bath
3. customWhile the resulting reaction mixture
4. filtrationThe resulting crystals were filtered off under pressure in a nitrogen gas atmosphere
5. washAfter the crystals were washed with anhydrous diethyl ether three times, they
6. distillationwere purified by vacuum-distillation (0.4 kPa, 77.8-78.2° C.)

ORDレコード

ord-e094eb63ae574f998603998d9ea6316b

出典データセット

uspto-grants-2014_10

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08871974B2