7-Methoxy-5-Methylbenzo[b]thiophene synthesis
- Product Name:7-Methoxy-5-Methylbenzo[b]thiophene
- CAS Number:1388033-29-1
- Molecular formula:C10H10OS
- Molecular Weight:178.25
1443531-59-6
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1388033-29-1
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Yield: 49%
Reaction Conditions:
with polyphosphoric acid in chlorobenzeneReflux;
Steps:
7-Methoxy-5-methyl-1-benzothiophene
To a refluxing mixture of 13 g polyphosphoric acid and 150 ml chlorobenzene was added dropwise a solution of 5.2 g (19.2 mmol) of Intermediate 3A, and refluxing was continued overnight. After cooling, the organic layer was decanted, and the residue and flask were rinsed twice with DCM. The combined organic phases were evaporated at reduced pressure. The residue (3.76 g) was chromato- graphed on silica gel with isohexane/0-10%> ethyl acetate as eluent. Yield: 1.69 g of an oil (49% of th.) GC-MS (method 6): Rt = 5.20 min; MS (EIpos): m/z = 178 (M)+ -NMR (400 MHz, DMSO-de): δ = 7.68 (d, 1H), 7.34 (d, 1H), 7.28 (s, 1H), 6.78 (s, 1H), 3.93 (s, 3H), 2.43 (s, 3H) ppm.
References:
Location in patent:Page/Page column 47
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