Diethyl Ether → HCID 22102064, compound

Temperature

0 °C

The inside of a 100 ml three-necked round-bottom flask, to which a dropping funnel is connected, was replaced with nitrogen, then a 1.0M diethyl ether solution (22 ml) of benzyl magnesium chloride was added and the mixture was cooled in an ice bath to 0° C. To this, carbon disulfide (1.32 ml) was dropped from a dropping funnel over 10 minutes, then the mixture was stirred at 0° C. for 4.5 hours. Thereafter, 30 ml of water was added, the mixture was returned to room temperature, the mixture was then washed with diethyl ether (total 100 ml) 2 times. Diethyl ether (50 ml) and 30% HCl (5 ml) were added and the product was extracted from the organic layer. Thereafter, the product was washed with water (total 150 ml) 3 times. The diethyl ether layer was concentrated to obtain phenylethyl dithiocarboxylic acid (1.86 g).

1. customThe inside of a 100 ml three-necked round-bottom flask, to which a dropping funnel is connected
2. customwas returned to room temperature
3. washthe mixture was then washed with diethyl ether (total 100 ml) 2 times
4. additionDiethyl ether (50 ml) and 30% HCl (5 ml) were added
5. extractionthe product was extracted from the organic layer
6. washThereafter, the product was washed with water (total 150 ml) 3 times
7. concentrationThe diethyl ether layer was concentrated

ORD record

ord-93821316a4914398b3a83417c4ba8b6f

Source dataset

uspto-grants-2014_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08796386B2