Chloride → 2-Chloro-4-isopropylthiazole

Temperatur

65 °C

500 mg of 4-isopropyl-thiazol-2-yl amine obtained in step 93-2 was dissolved in 10 ml of acetonitrile and 900 mg of cupper(II) chloride dehydrate was added to the mixture, followed by adding 630 μl of t-BuNO2 thereto dropwise. The resulting mixture was heated to 65° C. and stirred for 2 hr. The resulting solution was cooled to room temperature and the reaction was terminated by adding water. The resulting mixture was extracted twice with ethyl acetate and washed with water and saline solution. The organic layer was dried over anhydrous magnesium sulfate and concentrated under a reduced pressure to obtain 500 mg of the title compound as a light brown oil.

1. temperatureThe resulting solution was cooled to room temperature
2. customthe reaction was terminated
3. additionby adding water
4. extractionThe resulting mixture was extracted twice with ethyl acetate
5. washwashed with water and saline solution
6. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
7. concentrationconcentrated under a reduced pressure

ORD-Eintrag

ord-989034aef44d4a24886abe4356d9e010

Quelldatensatz

uspto-grants-2014_10

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08853213B2