Chloroform → 2-Benzothiazolamine, 4-chloro-

Temperatur

0 °C

The phenylthiourea (6.00 g, 32.16 mmol) was dissolved in CHCl3 (150 mL) and cooled to 0° C. with an ice bath. To this mixture was added a solution of Br2 (1.6 mL, 32.2 mmol) in CHCl3 (100 mL) dropwise over 30 min. After the addition, the mixture was stirred at 0° C. for 1 h, then allowed to warm to rt. the reaction was refluxed for 3 h to 4 h than allowed to cool to room temperature. The organic solvent was removed and the residue was washed with sulfurous acid. The residue was then neutralized with liquid ammonia. The solid was filtered off, washed with watyer and recrystallized from EtOH.

1. additionAfter the addition
2. temperatureto warm to rt
3. temperaturethe reaction was refluxed for 3 h to 4 h
4. temperatureto cool to room temperature
5. customThe organic solvent was removed
6. washthe residue was washed with sulfurous acid
7. filtrationThe solid was filtered off
8. washwashed with watyer
9. customrecrystallized from EtOH

ORD-Eintrag

ord-14f9242d6ba64935a248220f71c35a5b

Quelldatensatz

uspto-grants-2014_06

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08759336B2