Reaktion #579406

Reaktionsgleichung

4-phenylbenzo[b]thiophene

methacrylic acid

→

2-methyl-8-phenyl-1,2-dihydrobenzo[b]cyclopenta[d]thiophen-3-one

Lösungsmittel

dichloromethane

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.DISSOLUTIONhad completely dissolved
2. 2
   ExtraktionThe aqueous phase was extracted twice with 400 ml each time of a dichloromethane/hexane solvent mixture (30/70 parts by volume)

Vorschrift

A solution of 76.2 g of 4-phenylbenzo[b]thiophene (0.36 mol) and 37.5 ml of methacrylic acid (0.44 mol) in 50 ml of dichloromethane was added dropwise to 1000 g of super-PPA heated to 80° C. and stirred at 80° C. for 5 hours. The dark red mixture was added to 1000 g of crushed ice and stirred until the polyphosphoric acid had completely dissolved. The aqueous phase was extracted twice with 400 ml each time of a dichloromethane/hexane solvent mixture (30/70 parts by volume). The GC-MS. of the organic phase showed only starting product and no trace of the desired product.

Quelle