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Volumn 26, Issue 18, 2007, Pages 4386-4388

Formation of a double-bicapped hexatin phosphate cage by a de-arylation reaction. Synthesis and structure of [(PhSn)6(μ-OH) 2(μ-OEt)4{(ArO)PO3}4] (Ar = 2,6-i-Pr2C6H3)

(3) Chandrasekhar, Vadapalli a Sasikumar, Palani a Thilagar, Pakkirisamy a

a INDIAN INSTITUTE OF TECHNOLOGY KANPUR (India)

Author keywords

[No Author keywords available]

Indexed keywords

CHEMICAL BONDS; SYNTHESIS (CHEMICAL); TIN OXIDES;

CLEAVAGE; DE-ARYLATION REACTION; DOUBLE-BICAPPED HEXANUCLEAR MONOORGANOOXOTIN CAGE;

PHOSPHATES;

EID: 34548572953 PISSN: 02767333 EISSN: None Source Type: Journal
DOI: 10.1021/om700421b Document Type: Article

Times cited : (32)

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- Synthesis of 1: A mixture of ArP(O)2(OH)2 (0.25 g, 0.97 mmol) and (Ph3Sn)2O (0.69 g, 0.97 mmol) was taken in 80 mL of dry toluene and 5 mL of ethanol. The final mixtures were heated to reflux under dry nitrogen atmosphere for 4 h. The solvent was removed in vacuo to afford a sticky white solid, which was treated with dichloromethane (2 × 5 mL, and the solvent was removed to obtain the white solid, which upon recrystallization from a dry ethanol and dichloromethane mixture at room temperature by slow evaporation yielded colorless crystals suitable for X-ray analysis. Yield: 0.52 g (88, based on ArOPO3H2, mp 173-175 °C; 1H NMR (ppm) 0.71(m, 3.70(m, 3.30(m, and 7.19(m, 31P NMR (ppm) 1.98 (s, with 117/119Sn safellites and -17.26 (s, with 117/119Sn satellites, 119Sn NMR (CDCl3, ppm, 590.0 (dd, J[Sn-O-P, 102.8 Hz, 257.7 Hz) and -607.9
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