Methacrylic Acid → HCID 57679347, compound
Reaction equation
[C:1]1([C:7]2[C:15]3[CH:14]=[CH:13][S:12][C:11]=3[CH:10]=[CH:9][CH:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[C:16](O)(=[O:20])[C:17]([CH3:19])=[CH2:18]>ClCCl>[CH3:18][CH:17]1[CH2:19][C:14]2[C:15]3[C:7]([C:1]4[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=4)=[CH:8][CH:9]=[CH:10][C:11]=3[S:12][C:13]=2[C:16]1=[O:20]Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 80 °C
Procedure
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.
Workup
- dissolutionhad completely dissolved
- extractionThe aqueous phase was extracted twice with 400 ml each time of a dichloromethane/hexane solvent mixture (30/70 parts by volume)
Sources & evidence
- ORD record
- ord-cf4d07715126462882a66cc9d8537dd1
- Source dataset
- uspto-grants-2009_05
- Patent number
- US07531672B2
Reaction notes
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