ChemicalBook CAS DataBase List Benzo[b]thiophen-10-methoxycycloheptanone

Benzo[b]thiophen-10-methoxycycloheptanone synthesis

3synthesis methods

Product Name:Benzo[b]thiophen-10-methoxycycloheptanone
CAS Number:59743-84-9
Molecular formula:C14H10O2S
Molecular Weight:242.29

67-56-1 Synthesis

67-56-1
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$7.29/5ml-f

9,10-DIBROMO-9,10-DIHYDRO-4H-BENZO(4,5)CYCLOHEPTA(1,2-B)THIOPHENE-4-ONE

34580-10-4
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Benzo[b]thiophen-10-methoxycycloheptanone

59743-84-9
101 suppliers
$49.00/100mg

Yield: 59.59%

Reaction Conditions:

Stage #1:methanol;9,10-dibromo-9,10-dihydro-4H-benzo<4,5>cyclohepta<1,2-b>thiophene-4-one in water for 4 h;Reflux;
Stage #2: with K₂O/MgO in water for 4 h;Reflux;Reagent/catalyst;

Steps:

1.2 (2) Methoxylation
Weighed 9,10-dihydro-9,10-dibromo-4H-benzo[4,5]cycloheptatriene[1,2-b]thiazol-4-one 29.2 g (0.1 mol) and 500 ml Mix water and methanol, stir and reflux for 4 hours, then add 1.1g of the K2O/MgO catalyst prepared in step (1) (the mass of the used catalyst is 3.8% of the raw material mass).After refluxing for 4 hours, after the reaction is complete, the reaction solution is filtered, the filter cake is washed with deionized water for 3 to 5 times, and dried to obtain the recovered solid base catalyst. The filtrate is concentrated under reduced pressure to about 100 ml (20% of the original volume). Cool to about 0 °C, stir and crystallize for 30 min, and filter.The filter cake was added to 400 ml of ethylene glycol monomethyl ether, and the temperature was raised to 95° C. and stirred for 30 minutes. Then, the mixture was cooled to about 0° C., stirred and crystallized for 1 hour, filtered and dried.Obtained yellow needle crystals 10-methoxy-4H-benzo[4,5]cycloheptatriene, 1,2-b]thiazol-4-one 17.4 g,The mass yield (based on the weight of 9,10-dihydro-9,10-dibromo-4Hbenzo[4,5]cyclohepta[1,2-b]thiazol-4-one) is about 59.59%. Content ≥97%, melting point 162-165°C.

References:

Zhejiang University of Technology;Pei Wen;Yang Tao;Sun Li;Wang Haibin;Yang Zhenping CN104817532, 2017, B Location in patent:Paragraph 0023; 0029-0030

1622-55-5 Synthesis

4-Oxo-9,10-dihydro-4H-benzo(4,5)-cyclohepta-(1,2b)thiophene

1622-55-5
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$65.00/1 g

59743-84-9
101 suppliers
$49.00/100mg

References

34580-10-4
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59743-84-9
101 suppliers
$49.00/100mg

4H-Benzo[4,5]cyclohepta[1,2-b]thiophen-4-one, 9-methoxy-

126939-24-0
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References

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