Water → 2-Hydroxyethyl cycloheptyl sulfide

2.32 g of 2-mercaptoethanol, dissolved beforehand in 10 cm3 of dimethylformamide, were slowly added, under an inert atmosphere and at a temperature in the region of 20° C., to a stirred suspension of 0.91 g of 60% sodium hydride in 10 cm3 of anhydrous dimethylformamide. After stirring for 20 minutes, 3.5 g of bromocycloheptane, dissolved in 10 cm3 of dimethylformamide, were added. The reaction was brought to completion by stirring at a temperature in the region of 20° C. for 1 hour 30 minutes. The reaction mixture was poured onto 150 cm3 of water to which have been added 100 cm3 of diethyl ether. The ethereal phase was separated by settling and the aqueous phase was extracted once with 50 cm3 of diethyl ether. The organic phases were combined and then washed with 2 times 100 cm3 of water, dried over magnesium sulfate, filtered, and concentrated under reduced pressure (5 kPa) at a temperature in the region of 40° C. 3.2 g of 2-hydroxyethyl cycloheptyl sulfide were obtained in the form of an oil with a yellow color.

1. additionwere added
2. stirringby stirring at a temperature in the region of 20° C. for 1 hour 30 minutes
3. customThe ethereal phase was separated
4. extractionthe aqueous phase was extracted once with 50 cm3 of diethyl ether
5. washwashed with 2 times 100 cm3 of water
6. dry with materialdried over magnesium sulfate
7. filtrationfiltered
8. concentrationconcentrated under reduced pressure (5 kPa) at a temperature in the region of 40° C

ORDレコード

ord-c15893eda1a044219750fd1658c36fda

出典データセット

uspto-grants-2002_06

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US06403610B1