تفاعل #577203

ord-a644f2565aec45988e51953c9e35ac4f

معادلة التفاعل

C#Cc1ccc(N)cc1
4-ethynylaniline
CCN(CC)CC
triethylamine
C#Cc1ccc(N)cc1
4-ethynylaniline
Ic1ccc(I)cc1
1,4-Diiodobenzene
Nc1ccc(C#Cc2ccc(I)cc2)cc1
desired product
Nc1ccc(C#Cc2ccc(I)cc2)cc1
4-(4-Iodophenylethynyl)Aniline

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىThe tube was capped

الإجراء التجريبي

1,4-Diiodobenzene (4.95 g, 1.0 mmol), bis(triphenylphosphine)palladium(II) dichloride (0.070 g, 0.10 mmol), copper(I) iodide (0.019 g, 0.10 mmol), triethylamine (5 mL), THF (10 mL) and 4-ethynylaniline 0.585 g, 5.00 mmol) were used following the general procedure for couplings. For the synthesis of 4-ethynylaniline, please see Tour et al. Chem. Eur. J. 2001, vol. 7, pp. 5118-5134 incorporated herein by reference. The tube was capped and stirred room temperature for 12 h. Flash column chromatography (CH2Cl2—hexanes as eluent) afforded the desired product as light yellow needles (1.13 g, 71% yield). IR (KBr) 3441, 3356, 2210, 1612, 1515, 1281, 1135, 1003, 842, 811, 512 cm−1. 1H NMR (400 MHz, CDCl3) δ7.650 (m, AA′ part of AA‘XX’ pattern, J=8.7, 2.4, 1.8, 0.7 Hz, 2H), 7.324 (m, XX′ part of AA′XX′ pattern, J=8.7, 2.4, 1.8, 0.7 Hz, 2H), 7.208 (m, AA′ part of AA′XX′ pattern, J=8.6, 2.4, 1.8, 0.6 Hz, 2H), 6.630 (m, XX′ part of AA′XX′ pattern, J=8.6, 2.4, 1.8, 0.6 Hz, 2H), 3.833 (s, 2H). 13C NMR (100 MHz, CDCl3) δ 147.05, 137.60, 133.20, 133.07, 123.67, 114.95, 112.39, 93.45, 91.83, 86.69.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07527831B2uspto-grants-2009_05