تفاعل #992760

معادلة التفاعل

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

bis-(2-chloroethyl)ether

sodium iodide

→

title compound

المردود 24.0%

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

المردود 24.0%

المذيبات

acetonitrile

ظروف التفاعل

المعالجة

1. 1
   تركيزThe crude mixture was concentrated in vacuo
2. 2
   workup.DISSOLUTIONredissolved in ethyl acetate (100 mL)
3. 3
   غسيلwashed with water (2×100 mL) and brine (1×100 mL)
4. 4
   تجفيفThe organic phase was dried over magnesium sulfate
5. 5
   تركيزconcentrated in vacuo
6. 6
   أخرىThe crude product was purified by flash chromatography

الإجراء التجريبي

2-Chloro-6-trifluoromethyl-benzene-1,4-diamine (2.9 g), bis-(2-chloroethyl)ether (1.7 mL) and sodium iodide (516 mg) were mixed in acetonitrile (45 mL) and heated to 165° C. for 1 hour in a sealed microwave process vessel. The crude mixture was concentrated in vacuo, redissolved in ethyl acetate (100 mL) and washed with water (2×100 mL) and brine (1×100 mL). The organic phase was dried over magnesium sulfate and concentrated in vacuo. The crude product was purified by flash chromatography to furnish 940 mg (24%) of the title compound as a black oil. 1H NMR (500 MHz, CDCl3): 3.02 (m, 4H), 3.84 (m, 4H), 4.30 (b, 2H), 6.97 (d, 1H), 7.06 (d, 1H).

المصدر