تفاعل #510626

معادلة التفاعل

tin(II)chloride dihydrate

9,10-bis-(4-bromo-phenylethynyl)-9,10-dihydro-anthracene-9,10-diol

→

title compound

9,10-Bis-(4-bromo-phenylethynyl)anthracene

المذيبات

water

acetic acid

aceton

ظروف التفاعل

المعالجة

1. 1
   workup.ADDITIONis added within 15 minutes
2. 2
   ترشيحthe solid is filtered off

الإجراء التجريبي

To a suspension of 9,10-bis-(4-bromo-phenylethynyl)-9,10-dihydro-anthracene-9,10-diol (2.0 g, 3.5 mmol) in aceton (25 ml), a solution of tin(II)chloride dihydrate (1.82 g, 8.05 mmol) in a mixture of water (15 ml) and acetic acid (15 ml) is added within 15 minutes. The obtained suspension is stirred for another 2.5 hours at ambient temperature, and then the solid is filtered off to give a first crop the title compound. Over night another crop of product crystallizes from the mother liquors, and the combined crops are recrystallized from anisol (30 ml) to give the title compound as orange needles. DSC: mp=305° C. MS: 534 (correct isotope pattern). Elementary analysis: C, 67.45; (calcd. 67.19); H, 3.23; (calcd. 3.01).

المصدر