Hydrochloric Acid → HCID 131729038, Verbindung

10 ml of methylene chloride, 2 g (9.4 mmol) of (S)-3-(2-methoxyphenylsulfanyl)-2-methylpropanol, 2 g (10.5 mmol) of para-toluenesulfonyl chloride and 115 mg (0.94 mmol) of 4-dimethylaminopyridine are introduced into a three-necked flask under an inert atmosphere and 1.2 g (12.1 mmol) of triethylamine are then added dropwise. After stirring for 2 hours at ambient temperature, 10 ml of demineralised water are added. The pH is adjusted to 6.5 by adding 2N hydrochloric acid. The phases are separated and then the organic phase is washed with 10 ml of demineralised water. The organic phase is concentrated under reduced pressure. The yellow oil obtained (3.2 g) is taken up in a mixture of methylene chloride (4.8 ml) and 19.2 ml of isopropyl ether. The precipitate obtained is filtered off and then washed twice with 10 ml of isopropyl ether and dried at 40° C. under reduced pressure. The title product (3) is obtained in the form of a white powder 2.6 g (75%).

1. additionare then added dropwise
2. customThe phases are separated
3. washthe organic phase is washed with 10 ml of demineralised water
4. concentrationThe organic phase is concentrated under reduced pressure
5. customThe yellow oil obtained (3.2 g)
6. customThe precipitate obtained
7. filtrationis filtered off
8. washwashed twice with 10 ml of isopropyl ether
9. customdried at 40° C. under reduced pressure

ORD-Eintrag

ord-c1958916911947d2b39bea9b2c9a571e

Quelldatensatz

uspto-grants-2011_07

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07982054B2