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Volumn 13, Issue 8, 2010, Pages 988-991

Rhodium(III) complexes of N-{2-(arylseleno/telluro)ethyl} morpholine: Synthesis, structure and applications as efficient catalyst for transfer hydrogenation reaction of ketones

(4) Singh, Pradhumn a Das, Dipanwita a Singh, Monika a Singh, Ajai K a

a INDIAN INSTITUTE OF TECHNOLOGY DELHI (India)

Author keywords

Catalytic transfer hydrogenation; Crystal structure; Ketone; Rhodium(III); Selenium; Tellurium

Indexed keywords

EID: 77953912581 PISSN: 13877003 EISSN: None Source Type: Journal
DOI: 10.1016/j.inoche.2010.05.014 Document Type: Article

Times cited : (11)

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- General procedure for synthesis of ligands L1 and L2: Diphenyldiselenide (0.62 g, 2.0 mmol)/bis(4-methoxyphenyl)ditelluride (0.94 g, 2 mmol) dissolved in 30 cm3 of ethanol was reacted with solution (added drop wise) of NaBH4 (0.14 g, 4.0 mmol) in NaOH (5, under N2 atmosphere at room temperature (for L1) or under refluxing (for L2, The resulting PhSeNa/ArTeNa. was treated with 4-(2-chloroethyl)morpholine hydrochloride (0.74 g, 4.0 mmol) dissolved in 5 cm3 of ethanol with constant stirring. The reaction mixture further stirred for 3-4 h was poured into ice cold water (20 cm3) containing 0.2 g of NaOH. The ligand L1 or L2 was extracted into CHCl3 (5 × 40 cm3, The extract was washed with water (3 × 50 cm3) and dried over anhydrous sodium sulphate. On evaporating off chloroform under reduced pressure on rotary evaporator L1/L2 was obtained as oil (L1: pale yellow; L2: white) L1: Yield 0.8
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- General procedure for synthesis of complexes [RhCl2(L1)4, 61481;[ClO4, 1) and [RhCl2(L2)4][ClO4, 2)·C2H5OH·2H2O: The mixture of ethanolic solution (20 cm3) of RhCl3·3H2O (0.053 g, 0.2 mmol) and a solution of L1/L2 (0.054/0.070 g, 0.2 mmol) made in C2H5OH (7 cm3) was stirred for 3-4 h, followed by addition of AgClO4 (0.042 g, 0.2 mmol) in C2H5OH (5 cm3) till it became orange for 1 and red for 2. The AgCl was filtered off. The of filtrate was reduced to ∼ 7 cm3 on a rotary evaporator. The addition of diethyl ether (15 cm3) to the concentrate gave 1 (orange) and 2 (red) as precipitate which was filtered, washed with diethyl ether (10 cm3) and dried in vacuo. Single crystals of 2 suitable for X-ray diffraction were ob
- 125Te) 53.1 Hz).

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- - 3] 1.632/-0.977.
- - 3] 1.632/-0.977.

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- o): Cl(1)-Rh(1)-Cl(2) 178.26(7), Cl(1)-Rh(1)-Te(1) 91.27(5), Cl(1)-Rh(1)-Te(2) 86.63(5), Cl(1)-Rh(1)-Te(3) 92.03(5), Cl(1)-Rh(1)-Te(4) 90.18(5), Cl(2)-Rh(1)-Te(1) 88.53(5), Cl(2)-Rh(1)-Te(2) 91.66(5), Cl(2)-Rh(1)-Te(3) 88.25(5), Cl(2)-Rh(1)-Te(4) 91.53(5), Te(1)-Rh(1)-Te(2) 92.49(3), Te(1)-Rh(1)-Te(3) 175.85(3), Te(1)-Rh(1)-Te(4) 87.94(2), Te(2)-Rh(1)-Te(3) 90.20(2), Te(2)-Rh(1)-Te(4) 176.79(3), Te(3)-Rh(1)-Te(4) 89.54(2).
- o): Cl(1)-Rh(1)-Cl(2) 178.26(7), Cl(1)-Rh(1)-Te(1) 91.27(5), Cl(1)-Rh(1)-Te(2) 86.63(5), Cl(1)-Rh(1)-Te(3) 92.03(5), Cl(1)-Rh(1)-Te(4) 90.18(5), Cl(2)-Rh(1)-Te(1) 88.53(5), Cl(2)-Rh(1)-Te(2) 91.66(5), Cl(2)-Rh(1)-Te(3) 88.25(5), Cl(2)-Rh(1)-Te(4) 91.53(5), Te(1)-Rh(1)-Te(2) 92.49(3), Te(1)-Rh(1)-Te(3) 175.85(3), Te(1)-Rh(1)-Te(4) 87.94(2), Te(2)-Rh(1)-Te(3) 90.20(2), Te(2)-Rh(1)-Te(4) 176.79(3), Te(3)-Rh(1)-Te(4) 89.54(2).

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