تفاعل #992749

معادلة التفاعل

bicarbonate

2-Bromo-6-trifluoromethyl-benzene-1,4-diamine

bis-(2-bromoethyl)ether

N,N-diisopropyl-ethylamine

→

title compound

المردود 63.0%

2-Bromo-4-morpholin-4-yl-6-trifluoromethyl-phenylamine

المردود 63.0%

المذيبات

N,N-dimethylformamide

ظروف التفاعل

المعالجة

1. 1
   استخلاصthe crude mixture was extracted with ethyl acetate (100 mL)
2. 2
   غسيلThe organic phase was washed with water (100 mL) and brine (100 mL)
3. 3
   تجفيفdried over sodium sulfate
4. 4
   تركيزconcentrated in vacuo
5. 5
   أخرىThe crude product was purified by flash chromatography

الإجراء التجريبي

2-Bromo-6-trifluoromethyl-benzene-1,4-diamine (2.21 g), bis-(2-bromoethyl)ether (1.30 mL) and N,N-diisopropyl-ethylamine (4.64 mL) were mixed in N,N-dimethylformamide (19 mL) and heated to 180° C. for 30 minutes in a sealed microwave process vial. Saturated aqueous bicarbonate (100 mL) was added and the crude mixture was extracted with ethyl acetate (100 mL). The organic phase was washed with water (100 mL) and brine (100 mL), dried over sodium sulfate and concentrated in vacuo. The crude product was purified by flash chromatography to furnish 1.78 g (63%) of the title compound as a yellow solid. LC-MS (m/z) 326 (MH+); tR=2.54, (UV, ELSD) 83%, 75%. 1H NMR (500 MHz, DMSO-d6): 2.99 (m, 4H), 3.70 (m, 4H), 5.00 (s, 2H), 7.00 (d, 1H), 7.38 (d, 1H).

المصدر