Ethyl benzo[d][1,3]dioxole-4-carboxylate synthesis
- Product Name:Ethyl benzo[d][1,3]dioxole-4-carboxylate
- CAS Number:23158-06-7
- Molecular formula:C10H10O4
- Molecular Weight:194.18
75-09-2
1262 suppliers
$10.00/25ML
3943-73-5
70 suppliers
$16.00/100mg
23158-06-7
6 suppliers
inquiry
Yield:23158-06-7 68%
Reaction Conditions:
with potassium fluoride in N,N-dimethyl-formamide at 110; for 14.5 h;
Steps:
68.2
To a solution of the compound of the previous step (22 g) in DMF (200 ml) were added potassium fluoride (36 g) and CH2Cl2 (9.0 ml), and the mixture was stirred at 110°C for 8 hr. CH2Cl2 (20 ml) was added to the solution, and the mixture was further stirred at 110°C for 6.5 hr. The reaction solution was poured into water, and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine, and dried over magnesium sulfate. The solvent was evaporated under reduced pressure. The residue was subjected to normal phase chromatography (elution solvent hexane-ethyl acetate=4:1) to give the title compound (16 g, 68%). NMR(300MHz, CDCl3)δ:1.39(3H, t, J=7.2Hz), 4.39(2H, q, J=7.2Hz), 6.10(2H, s), 6.86(1H, dd, J=8.1, 7.2Hz), 6.97(1H, dd, J=7.2, 1.2Hz), 7.41(1H, dd, J=8.1, 1.2Hz).
References:
EP2116538,2009,A1 Location in patent:Page/Page column 49
5768-39-8
110 suppliers
$54.00/100mg
64-17-5
824 suppliers
$10.00/50g
23158-06-7
6 suppliers
inquiry
303-38-8
333 suppliers
$15.00/5g
23158-06-7
6 suppliers
inquiry
2411-83-8
112 suppliers
$13.00/1g
23158-06-7
6 suppliers
inquiry
33842-16-9
89 suppliers
$45.00/100mg
23158-06-7
6 suppliers
inquiry