تفاعل #9672

معادلة التفاعل

2-chloro-4-trifluoromethylaniline

potassium O-ethyl dithiocarbonate

HCl

→

desired product

المردود 99.0%

2-Chloro-6-(trifluoromethyl)benzothiazole

المردود 99.0%

المذيبات

DMF

ظروف التفاعل

المعالجة

1. 1
   أخرىprecipitation
2. 2
   workup.STIRRINGAfter the mixture was stirred for 30 minutes
3. 3
   ترشيحthe solid precipitate was collected by filtration
4. 4
   غسيلrinsed with water
5. 5
   workup.DISSOLUTIONThe filter cake was dissolved in 100 mL EtOAc
6. 6
   تجفيفthe solution was dried over Na2SO4
7. 7
   أخرىEtOAc was removed by rotary evaporation
8. 8
   أخرىthe residue was dried in vacuo

الإجراء التجريبي

A mixture of 2-chloro-4-trifluoromethylaniline (15.0 g, 76.7 mmol) and potassium O-ethyl dithiocarbonate (29.5 g, 184.1 mmol) in 75 mL anhydrous.DMF was heated at 130° C. overnight under a nitrogen atmosphere. The reaction mixture was cooled to rt, and then 1 N HCl solution (200 mL) was added with stirring to induce precipitation. After the mixture was stirred for 30 minutes, the solid precipitate was collected by filtration and rinsed with water. The filter cake was dissolved in 100 mL EtOAc, and the solution was dried over Na2SO4. EtOAc was removed by rotary evaporation, and the residue was dried in vacuo to afford the desired product as a white solid (18.0 g, 99%). 1H NMR (DMSO-d6) δ 14.00 (bs, 1 H), 8.20 (s, 1 H), 7.70 (d, 1 H), 7.40 (d, 1 H); GC-EIMS m/z 235 (M+).

المصدر